CN116713464B - Super wear-resistant nano powder alloy material and preparation method thereof - Google Patents
Super wear-resistant nano powder alloy material and preparation method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 101
- 239000011858 nanopowder Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 108
- 229910001199 N alloy Inorganic materials 0.000 claims abstract description 99
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 93
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910018540 Si C Inorganic materials 0.000 claims abstract description 34
- GQLSFFZMZXULSF-UHFFFAOYSA-N copper;oxotungsten Chemical compound [Cu].[W]=O GQLSFFZMZXULSF-UHFFFAOYSA-N 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000000975 co-precipitation Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 239000011812 mixed powder Substances 0.000 claims description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- AZAKMLHUDVIDFN-UHFFFAOYSA-N tert-butyl nitrate Chemical compound CC(C)(C)O[N+]([O-])=O AZAKMLHUDVIDFN-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000009423 ventilation Methods 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- -1 alkyl orthosilicate Chemical compound 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005273 aeration Methods 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 44
- 238000000151 deposition Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 230000006872 improvement Effects 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229910000640 Fe alloy Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910000611 Zinc aluminium Inorganic materials 0.000 description 3
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910000906 Bronze Inorganic materials 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a super wear-resistant nano powder alloy material and a preparation method thereof, and belongs to the technical field of alloys. Treating superfine iron powder with ammonia gas to obtain nanometer Fe-N alloy powder, adding the nanometer Fe-N alloy powder into Si-C sol, drying, calcining to obtain nanometer Fe-N alloy powder coated with SiC, adding the nanometer Fe-N alloy powder into acid solution containing copper nitrate and ammonium tungstate to perform coprecipitation reaction, calcining to obtain nanometer Fe-N alloy powder coated with SiC, depositing tungsten copper oxide, and reducing with low-temperature hydrogen to obtain the ultra-wear-resistant nanometer powder alloy material. The super wear-resistant nano powder alloy material prepared by the invention has extremely strong strength, extremely good wear resistance, high heat conduction performance and high temperature resistance, uniform and compact tissue structure and excellent comprehensive performance, and the alloy material is mutually soluble, greatly improves the performance and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a super wear-resistant nano powder alloy material and a preparation method thereof.
Background
The wear-resistant alloy material is widely applied to key parts of industrial equipment such as electric power, metallurgy, cement, building materials, chemical industry and the like and bears abrasive wear. Frictional wear between workpieces is a primary mode of failure of relatively moving workpieces. In the occasion of long-term continuous operation, the heat generated by friction between the workpieces can raise the temperature of the friction surface of the workpieces, so that the working environment is more severe. Wear resistant alloys are the alloys developed to improve wear resistance of mechanical devices and some of the most commonly used alloys for typical friction pairs. The alloy has wide application, including various tool steels, bearing steels, high manganese steels for rock drilling and crushing machines and various wear-resistant cast irons.
In the prior art, the wear-resistant alloy used in the same occasion has smaller proportion difference between raw materials and basically similar strength, but has larger wear resistance difference, and part of wear-resistant alloy has poorer wear resistance, and the working environment is bad, so the alloy is easy to damage and even can be scrapped.
Chinese patent CN1015914B relates to a high-aluminum zinc-based wear-resistant alloy instead of tin bronze, which is used as alloy material for wear-resistant parts such as bearing bush, shaft sleeve, worm gear, etc. working under different working conditions in mechanical industry. The alloy comprises the following components in percentage by weight: 53% of zinc, 43% of aluminum, 3.5% of copper, 0.8% of silicon and 0.03% of magnesium. The alloy structure is that hard particles are distributed on a soft matrix, so that the wear resistance of the alloy is greatly improved, and the alloy has higher strength and hardness. Compared with tin bronze alloy, the zinc-based wear-resistant alloy in the application replaces copper with zinc, improves the aluminum content, reduces the weight of the alloy by 1/2 and reduces the cost by 50 percent, and is an ideal wear-resistant alloy material for sliding bearings.
Chinese patent CN100400692C relates to a zinc-aluminium base wear-resistant alloy material and its preparation method. The alloy material takes zinc-aluminum alloy as a matrix and contains silicon, tellurium or lanthanum, the bloom-shaped silicon phase is uniformly distributed on the zinc-aluminum alloy matrix, the shape silicon phase is self-generated in alloy liquid, the microscopic morphology of the silicon phase is bulk cracking polycrystal, and the alloy material comprises the following chemical components in percentage by weight: 40-50% of aluminum, 0.02-0.05% of tellurium or lanthanum, 1.0-3.0% of silicon and the balance of zinc.
The invention has limited improvement of wear resistance and heat resistance due to low silicon content.
Disclosure of Invention
The invention aims to provide a super wear-resistant nano powder alloy material and a preparation method thereof, which have extremely strong strength, extremely good wear resistance, high heat conduction performance and high temperature resistance, uniform and compact tissue structure and excellent comprehensive performance, and the alloy material is mutually soluble, greatly improves the performance and has wide application prospect.
The technical scheme of the invention is realized as follows:
the invention provides a preparation method of a super wear-resistant nano powder alloy material, which comprises the steps of treating superfine iron powder with ammonia gas to prepare nano Fe-N alloy powder, adding the nano Fe-N alloy powder into Si-C sol, drying, calcining to prepare nano Fe-N alloy powder coated with SiC, adding the nano Fe-N alloy powder into an acidic solution containing copper nitrate and ammonium tungstate to perform coprecipitation reaction, calcining to prepare nano Fe-N alloy powder coated with SiC, depositing tungsten copper oxide, and reducing with low-temperature hydrogen to obtain the super wear-resistant nano powder alloy material.
As a further improvement of the invention, the method comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 550-650 deg.c, cooling to room temperature and ball milling to obtain nanometer Fe-N alloy powder;
s2, preparation of Si-C sol: dissolving alkyl orthosilicate and methyl methacrylate in ethanol, adding tert-butyl nitrate at room temperature under the protection of inert gas, stirring and mixing uniformly, adding dilute hydrochloric acid, and stirring until Si-C sol is formed;
s3, preparing SiC-coated nano Fe-N alloy powder: adding the nano Fe-N alloy powder prepared in the step S1 into the Si-C sol prepared in the step S2, uniformly stirring and mixing, drying, calcining, and ball-milling to prepare nano Fe-N alloy powder coated with SiC;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding concentrated nitric acid into a copper nitrate solution to prepare solution A, adding the SiC-coated nano Fe-N alloy powder prepared in the step S3 into an ammonium tungstate solution, carrying out ultrasonic mixing uniformly to prepare suspension B, adding the solution A into the suspension B, stirring to carry out coprecipitation reaction, centrifuging, ball-milling and roasting to prepare the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) reducing the nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide, which is prepared in the step (S4), by using low-temperature hydrogen to obtain the super wear-resistant nano powder alloy material.
As a further improvement of the present invention, powder of at least one of the following is added to the ball mill in step S1: copper powder, nickel powder, chromium powder, zinc powder and graphite powder; the ball milling time is 4-5h, the flow of ammonia gas treatment is 5-7L/min, the content of oxygen in the ammonia gas is 2-3wt% and the content of carbon dioxide is 1-2wt% and the treatment time is 2-3h.
As a further improvement of the invention, graphite powder and nickel powder are added in the ball mill, and the mass ratio is 5-7:2.
As a further improvement of the invention, in the step S2, the mass ratio of the alkyl orthosilicate, the methyl methacrylate, the ethanol, the tert-butyl nitrate and the diluted hydrochloric acid is 12-15:2-3:50-70:3-5:15-20, the concentration of the diluted hydrochloric acid is 1-2mol/L, and the time from stirring to forming the Si-C sol is 1-2h.
As a further improvement of the invention, the mass ratio of the nano Fe-N alloy powder to the Si-C sol in the step S3 is 5-7:12-15, the drying temperature is 80-90 ℃, the time is 1-2h, the calcining temperature is 1200-1300 ℃, the time is 3-5h, and the ball milling time is 2-3h.
As a further improvement of the invention, in the step S4, the mass ratio of the copper nitrate to the concentrated sulfuric acid is 2-3:10-12, the concentration of the concentrated sulfuric acid is 5.5-6mol/L, the mass ratio of the nano Fe-N alloy powder coated with SiC to the ammonium tungstate is 10-12:3-5, the coprecipitation reaction time is 0.5-1h, the roasting temperature is 250-350 ℃, the time is 2-3h, and the ball milling time is 1-2h.
As a further improvement of the invention, the low-temperature hydrogen is reduced to be introduced into the reactor for reduction for 2 to 4 hours at the temperature of 650 to 750 ℃ in the step S5, and the ventilation amount of the hydrogen is 13 to 15L/min.
As a further improvement of the invention, the method specifically comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 550-650 ℃ for 2-3h, wherein the flow rate of the ammonia gas is 5-7L/min, the ammonia gas contains 2-3wt% of oxygen and 1-2wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4-5h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 5-7wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 5-7:2;
s2, preparation of Si-C sol: dissolving 12-15 parts by weight of alkyl orthosilicate and 2-3 parts by weight of methyl methacrylate in 50-70 parts by weight of ethanol, adding 3-5 parts by weight of tert-butyl nitrate at room temperature under the protection of inert gas, stirring and mixing uniformly, adding 15-20 parts by weight of dilute hydrochloric acid, and stirring for 1-2 hours to form Si-C sol;
s3, preparing SiC-coated nano Fe-N alloy powder: adding 5-7 parts by weight of nano Fe-N alloy powder prepared in the step S1 into 12-15 parts by weight of Si-C sol prepared in the step S2, stirring and mixing uniformly, drying at 80-90 ℃ for 1-2h, calcining at 1200-1300 ℃ for 3-5h, and ball milling for 2-3h to prepare nano Fe-N alloy powder coated with SiC;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding 2-3 parts by weight of concentrated nitric acid with the concentration of 5.5-6mol/L into 100 parts by weight of aqueous solution containing 10-12 parts by weight of copper nitrate to prepare solution A, adding 10-12 parts by weight of nano Fe-N alloy powder coated with SiC and prepared in the step S3 into 100 parts by weight of aqueous solution containing 3-5 parts by weight of ammonium tungstate, uniformly mixing by ultrasonic waves to prepare suspension B, adding the solution A into the suspension B, stirring to perform coprecipitation reaction for 0.5-1h, centrifuging, ball-milling for 1-2h, and roasting at the temperature of 250-350 ℃ for 2-3h to prepare nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide and prepared in the step (S4) at 650-750 ℃ for reduction for 2-4h, wherein the ventilation amount of the hydrogen is 13-15L/min, and thus the ultra-wear-resistant nano powder alloy material is obtained.
The invention further protects the super wear-resistant nano powder alloy material prepared by the preparation method.
The invention has the following beneficial effects: the invention firstly reduces and nitrides the iron powder or directly keeps the temperature for a certain time under the high temperature of ammonia gas to obtain Fe-N alloy powder with higher nitrogen concentration, and the introduction of nitrogen element forms solid solution in the alloy, so that the strengthening effect is more obvious than that of carbon, and the tensile strength and hardness of the material can be obviously improved. Improving the plasticity of the iron alloy, reducing the brittleness and enhancing the toughness of the iron alloy, and simultaneously, being beneficial to improving the wear resistance and the cutting resistance of the iron alloy and improving the corrosion resistance.
In the ball milling process, ni and C elements are introduced by introducing nickel powder and graphite powder, so that fine crystal strengthening is generated on the alloy, and the strength and wear resistance of the alloy powder are improved; the introduction of Ni element can also improve the corrosion resistance of the alloy, prolong the service life of the alloy and improve the plasticity and toughness of the alloy, thereby enabling the alloy to be easier to process and form. The C element can also form carbide with higher hardness, and can play a better role in lubrication under friction conditions such as shearing, pressing and sliding, so that the wear resistance is improved, a stable heat treatment phase is formed, the heat resistance is improved, a fine grain structure is formed, and the conductivity is improved.
The carbon nanomaterial and the ceramic particles have excellent characteristics of high thermal conductivity, high Young's modulus, high mechanical strength and the like, siC is a compound with very strong covalent bonds, and the ionic property of Si-C bonds in SiC is only 12%, so that the SiC has high strength, large elastic modulus and excellent wear resistance and high temperature resistance. According to the invention, nano Fe-N alloy powder is introduced into Si-C sol through sol-gel reaction, and coated on the surface of the nano Fe-N alloy powder, gel is formed through drying, and then a SiC layer is coated on the surface of the nano Fe-N alloy powder through high-temperature calcination, so that the wear resistance and mechanical strength of the alloy powder are obviously improved.
The tungsten-copper composite material has excellent thermal and electrical properties, higher strength, higher hardness, lower thermal expansion coefficient and better corrosion resistance, a layer of tungsten-copper oxide is deposited on the surface of nano Fe-N alloy powder coated with SiC by a coprecipitation method, and a tungsten-copper alloy material is formed by hydrogen reduction, so that the nano powder alloy material containing W, cu, ni, C, N, fe is prepared.
The super wear-resistant nano powder alloy material prepared by the invention has extremely strong strength, extremely good wear resistance, high heat conduction performance and high temperature resistance, uniform and compact tissue structure and excellent comprehensive performance, and the alloy material is mutually soluble, greatly improves the performance and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is an SEM image of a super abrasive nano-powder alloy material prepared in example 1 of the present invention;
FIG. 2 is an optical microscopic structure chart of a sample of the alloy material produced in test example 1 of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Graphite powder, 1000 mesh, content >99%, purchased from the company of graphite, eastern Kaiki, qingdao; nickel powder with purity of >99.9% and average particle size of 50nm, purchased from Ningbo gold nano materials science and technology Co., ltd; superfine iron powder, 1000 meshes, with the content of >98%, is purchased from Hennuo metal processing factories in Huaian district of Huaian city.
Example 1
The embodiment provides a preparation method of a super wear-resistant nano powder alloy material, which specifically comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 550 ℃ for 2h, wherein the flow rate of the ammonia gas is 5L/min, the ammonia gas contains 2wt% of oxygen and 1wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 5wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder in a mass ratio of 5:2;
s2, preparation of Si-C sol: dissolving 12 parts by weight of methyl orthosilicate and 2 parts by weight of methyl methacrylate in 50 parts by weight of ethanol, adding 3 parts by weight of tert-butyl nitrate at room temperature under the protection of nitrogen, stirring and mixing for 30min, adding 15 parts by weight of 1mol/L dilute hydrochloric acid, and stirring for 1h to form Si-C sol;
s3, preparing SiC-coated nano Fe-N alloy powder: adding 5 parts by weight of the nano Fe-N alloy powder prepared in the step S1 into 12 parts by weight of the Si-C sol prepared in the step S2, stirring and mixing for 20min, drying at 80 ℃ for 1h, calcining at 1200 ℃ for 3h, and ball milling for 2h to prepare SiC-coated nano Fe-N alloy powder;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding 2 parts by weight of concentrated nitric acid with the concentration of 5.5mol/L into 100 parts by weight of aqueous solution containing 10 parts by weight of copper nitrate to prepare solution A, adding 10 parts by weight of nano Fe-N alloy powder coated with SiC and prepared in the step S3 into 100 parts by weight of aqueous solution containing 3 parts by weight of ammonium tungstate, carrying out ultrasonic mixing for 15min at 1000W to prepare suspension B, adding the solution A into the suspension B, stirring to carry out coprecipitation reaction for 0.5h, centrifuging for 15min at 3000r/min, carrying out ball milling for 1h, and roasting for 2h at 250 ℃ to prepare nano Fe-N alloy powder coated with SiC and deposited tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide and prepared in the step (S4) at 650 ℃ for reduction for 2 hours, wherein the ventilation amount of the hydrogen is 13L/min, and thus the super wear-resistant nano powder alloy material is obtained. Fig. 1 is an SEM image of the prepared super wear-resistant nano powder alloy material, and the particle size of the particles is mostly less than 100nm.
Example 2
The embodiment provides a preparation method of a super wear-resistant nano powder alloy material, which specifically comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 650 ℃ for 3h, wherein the flow rate of the ammonia gas is 7L/min, the ammonia gas contains 3wt% of oxygen and 2wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 5h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 7wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 7:2;
s2, preparation of Si-C sol: dissolving 15 parts by weight of tetraethoxysilane and 3 parts by weight of methyl methacrylate in 70 parts by weight of ethanol, adding 5 parts by weight of tert-butyl nitrate at room temperature under the protection of nitrogen, stirring and mixing for 30min, adding 20 parts by weight of 2mol/L dilute hydrochloric acid, and stirring for 2h to form Si-C sol;
s3, preparing SiC-coated nano Fe-N alloy powder: adding 7 parts by weight of the nano Fe-N alloy powder prepared in the step S1 into 15 parts by weight of the Si-C sol prepared in the step S2, stirring and mixing for 20min, drying at 90 ℃ for 2h, calcining at 1300 ℃ for 5h, and ball milling for 3h to prepare SiC-coated nano Fe-N alloy powder;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding 3 parts by weight of 6mol/L concentrated nitric acid into 100 parts by weight of aqueous solution containing 12 parts by weight of copper nitrate to prepare solution A, adding 12 parts by weight of nano Fe-N alloy powder coated with SiC and prepared in the step S3 into 100 parts by weight of aqueous solution containing 5 parts by weight of ammonium tungstate, carrying out ultrasonic mixing for 15min at 1000W to prepare suspension B, adding the solution A into the suspension B, stirring to carry out coprecipitation reaction for 1h, centrifuging for 15min at 3000r/min, ball-milling for 2h, and roasting for 3h at 350 ℃ to prepare nano Fe-N alloy powder coated with SiC and deposited tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide and prepared in the step (S4) at 750 ℃ for reduction for 4 hours, wherein the ventilation amount of the hydrogen is 15L/min, and obtaining the super wear-resistant nano powder alloy material.
Example 3
The embodiment provides a preparation method of a super wear-resistant nano powder alloy material, which specifically comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 600 ℃ for 2.5h, wherein the flow rate of the ammonia gas is 6L/min, the ammonia gas contains 2.5wt% of oxygen and 1.5wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4.5h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 6wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 6:2;
s2, preparation of Si-C sol: dissolving 13.5 parts by weight of tetraethoxysilane and 2.5 parts by weight of methyl methacrylate in 60 parts by weight of ethanol, adding 4 parts by weight of tert-butyl nitrate at room temperature under the protection of nitrogen, stirring and mixing for 30min, adding 17 parts by weight of 1.5mol/L dilute hydrochloric acid, and stirring for 1.5h to form Si-C sol;
s3, preparing SiC-coated nano Fe-N alloy powder: adding 6 parts by weight of the nano Fe-N alloy powder prepared in the step S1 into 13.5 parts by weight of the Si-C sol prepared in the step S2, stirring and mixing for 20min, drying at 85 ℃ for 1.5h, calcining at 1250 ℃ for 4h, and ball-milling for 2.5h to prepare the nano Fe-N alloy powder coated with SiC;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding 2.5 parts by weight of concentrated nitric acid with the concentration of 5.7mol/L into 100 parts by weight of aqueous solution containing 11 parts by weight of copper nitrate to prepare solution A, adding 11 parts by weight of nano Fe-N alloy powder coated with SiC and prepared in the step S3 into 100 parts by weight of aqueous solution containing 4 parts by weight of ammonium tungstate, carrying out ultrasonic mixing for 15min at 1000W to prepare suspension B, adding the solution A into the suspension B, stirring and carrying out coprecipitation reaction for 1h, centrifuging for 15min at 3000r/min, carrying out ball milling for 1.5h, and roasting at 300 ℃ for 2.5h to prepare nano Fe-N alloy powder coated with SiC and deposited tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide and prepared in the step (S4) at 700 ℃ for reduction for 3 hours, wherein the ventilation amount of the hydrogen is 14L/min, and thus the super wear-resistant nano powder alloy material is obtained.
Example 4
The difference compared to example 3 is that the mixed powder in step S1 comprises only a single graphite powder.
Example 5
The difference compared to example 3 is that the mixed powder in step S1 includes only a single nickel powder.
Comparative example 1
The difference compared with example 3 is that no mixed powder was added during the ball milling in step S1.
The method comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 600 ℃ for 2.5h, wherein the flow rate of the ammonia gas is 6L/min, the ammonia gas contains 2.5wt% of oxygen and 1.5wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4.5h to obtain the nano Fe-N alloy powder.
Comparative example 2
The difference from example 3 is that no ammonia treatment was used in step S1.
The method comprises the following steps:
s1, preparing nano Fe alloy powder: ball milling superfine iron powder for 4.5 hours, and adding mixed powder accounting for 6wt% of the total mass of the system in the ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 6:2, so as to prepare nano Fe alloy powder.
Comparative example 3
In comparison with example 3, the difference is that methyl methacrylate and t-butyl nitrate are not added in step S2.
The method comprises the following steps:
s2. Preparation of Si sol: 20 parts by weight of ethyl orthosilicate is dissolved in 60 parts by weight of ethanol, and under the protection of nitrogen, stirring and mixing are carried out for 30min at room temperature, 17 parts by weight of 1.5mol/L dilute hydrochloric acid is added, and stirring is carried out for 1.5h, so that Si sol is formed.
Comparative example 4
In comparison with example 3, the difference is that step S2 and step S3 are not performed.
The method comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 600 ℃ for 2.5h, wherein the flow rate of the ammonia gas is 6L/min, the ammonia gas contains 2.5wt% of oxygen and 1.5wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4.5h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 6wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 6:2;
s2, preparing nano Fe-N alloy powder for depositing tungsten copper oxide: adding 2.5 parts by weight of concentrated nitric acid with the concentration of 5.7mol/L into 100 parts by weight of aqueous solution containing 11 parts by weight of copper nitrate to prepare solution A, adding 11 parts by weight of nano Fe-N alloy powder prepared in the step S1 into 100 parts by weight of aqueous solution containing 4 parts by weight of ammonium tungstate, carrying out 1000W ultrasonic mixing for 15min to prepare suspension B, adding the solution A into the suspension B, stirring and carrying out coprecipitation reaction for 1h, centrifuging for 15min 3000r/min, ball-milling for 1.5h, and roasting for 2.5h at 300 ℃ to prepare nano Fe-N alloy powder for depositing tungsten copper oxide;
s3, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the nano Fe-N alloy powder for depositing tungsten copper oxide, which is prepared in the step (S2), and reducing for 3 hours at 700 ℃, wherein the ventilation amount of the hydrogen is 14L/min, so as to obtain the super wear-resistant nano powder alloy material.
Comparative example 5
In comparison with example 3, the difference is that steps S4 and S5 are not performed.
The method comprises the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 600 ℃ for 2.5h, wherein the flow rate of the ammonia gas is 6L/min, the ammonia gas contains 2.5wt% of oxygen and 1.5wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4.5h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 6wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 6:2;
s2, preparation of Si-C sol: dissolving 13.5 parts by weight of tetraethoxysilane and 2.5 parts by weight of methyl methacrylate in 60 parts by weight of ethanol, adding 4 parts by weight of tert-butyl nitrate at room temperature under the protection of nitrogen, stirring and mixing for 30min, adding 17 parts by weight of 1.5mol/L dilute hydrochloric acid, and stirring for 1.5h to form Si-C sol;
s3, preparing SiC-coated nano Fe-N alloy powder: adding 6 parts by weight of nano Fe-N alloy powder prepared in the step S1 into 13.5 parts by weight of Si-C sol prepared in the step S2, stirring and mixing for 20min, drying at 85 ℃ for 1.5h, calcining at 1250 ℃ for 4h, and ball milling for 2.5h to prepare nano Fe-N alloy powder coated with SiC, namely the super wear-resistant nano powder alloy material.
Test example 1
The super wear-resistant nano powder alloy materials prepared in examples 1-5 and comparative examples 1-5 are subjected to cold isostatic pressing under the pressure of 35MPa, then sintered at the temperature of more than 950 ℃ under nitrogen atmosphere, heat-preserved for 2 hours, cooled to below 800 ℃ under nitrogen atmosphere, discharged and cooled by water to prepare an alloy material sample, and as can be seen from the optical microscope tissue diagram of the prepared alloy material sample, the density of the alloy is higher. Performance testing was performed. The results are shown in Table 1.
The hardness of the alloy sample was measured with a Brinell hardness tester under a ram diameter of 5mm, a test load of 750kg and a dwell time of 30 s.
And carrying out friction and wear performance experiments at 900r/min by adopting an HRS-2M type high-speed reciprocating friction and wear testing machine. The ambient temperature is 25 ℃, the humidity is 50+/-5%, the time is 30min, and the friction load is 60N. Characterized by the volumetric wear rate, calculated as follows:
volume wear rate = V/(f×l)
Volume wear rate in mm 3 Nm; v represents the wear volume in mm 3 The method comprises the steps of carrying out a first treatment on the surface of the F represents a friction load, in N; l represents the total glide length in m.
The thermal conductivity of the alloy samples was measured with a thermal coefficient measuring instrument, and the dimensions of the alloy samples used were Φ10mm×3mm.
TABLE 1
| Group of | Hardness (HV) | Rate of volumetric wear (mm) 3 /Nm)×10 -8 | Thermal conductivity (W/m.K) |
| Example 1 | 472 | 1.3 | 212 |
| Example 2 | 477 | 1.1 | 214 |
| Example 3 | 480 | 1.0 | 215 |
| Example 4 | 469 | 7.9 | 205 |
| Example 5 | 467 | 8.5 | 204 |
| Comparative example 1 | 462 | 12.2 | 198 |
| Comparative example 2 | 456 | 13.7 | 202 |
| Comparative example 3 | 459 | 10.7 | 192 |
| Comparative example 4 | 442 | 22.4 | 187 |
| Comparative example 5 | 457 | 11.2 | 184 |
As can be seen from the above table, the super wear-resistant nano powder alloy material prepared in the embodiments 1-3 of the invention has the advantages of high hardness, better wear resistance and better thermal conductivity.
Test example 2
The super wear-resistant nano powder alloy materials prepared in the examples 1-5 and the comparative examples 1-5 are subjected to cold isostatic pressing under the pressure of 35MPa, then sintered at the temperature of more than 950 ℃ under nitrogen atmosphere, heat-preserved for 2 hours, cooled to below 800 ℃ under nitrogen atmosphere, discharged and cooled with water, and an alloy material sample is prepared, and the mechanical property test is carried out. The results are shown in Table 2.
The tensile strength of the alloy specimens was measured with an Instron3369 electronic tensile tester at a tensile rate of 1mm/min at room temperature.
And (3) carrying out a high-temperature tensile test on the AG-100KN material high-temperature performance tester, wherein the temperature rising rate is 10 ℃/min, the test temperature is 300-500 ℃, the heat preservation time is 20min, and the tensile rate is 1mm/min under the nitrogen atmosphere condition.
TABLE 2
As can be seen from the above table, the alloy materials prepared from the super wear-resistant nano powder alloy materials prepared in the embodiments 1-3 have better mechanical properties and better high temperature resistance.
Examples 4 and 5 in comparison with example 3, the mixed powder in step S1 includes only a single graphite powder or nickel powder. Comparative example 1 in comparison with example 3, no mixed powder was added during the ball milling in step S1. The wear resistance, mechanical property and high temperature resistance of the alloy are obviously reduced. In the ball milling process, ni and C elements are introduced by introducing nickel powder and graphite powder, so that fine crystal strengthening is generated on the alloy, and the strength and wear resistance of the alloy powder are improved; the introduction of Ni element can also improve the corrosion resistance of the alloy, prolong the service life of the alloy and improve the plasticity and toughness of the alloy, thereby enabling the alloy to be easier to process and form. The C element can also form carbide with higher hardness, and can play a better role in lubrication under friction conditions such as shearing, pressing and sliding, so that the wear resistance is improved, a stable heat treatment phase is formed, the heat resistance is improved, a fine grain structure is formed, and the conductivity is improved.
Comparative example 2 compared with example 3, no ammonia gas treatment was used in step S1. The wear resistance, mechanical property and hardness of the alloy are obviously reduced. The introduction of nitrogen element forms solid solution in alloy, and has obvious strengthening effect compared with carbon, and can raise the tensile strength and hardness of the material obviously. Improving the plasticity of the iron alloy, reducing the brittleness and enhancing the toughness of the iron alloy, and simultaneously, being beneficial to improving the wear resistance and the cutting resistance of the iron alloy and improving the corrosion resistance.
Comparative example 3 in contrast to example 3, methyl methacrylate and t-butyl nitrate were not added in step S2. In this comparative example, no SiC layer was formed, but SiO was formed 2 A layer. Comparative example 4 compared to example 3, steps S2 and S3 were not performed. The wear resistance, mechanical property, thermal conductivity and hardness of the alloy are obviously reduced. The carbon nanomaterial and the ceramic particles have excellent characteristics of high thermal conductivity, high Young's modulus, high mechanical strength and the like, siC is a compound with very strong covalent bonds, and the ionic property of Si-C bonds in SiC is only 12%, so that the SiC has high strength, large elastic modulus and excellent wear resistance and high temperature resistance. According to the invention, nano Fe-N alloy powder is introduced into Si-C sol through sol-gel reaction, and coated on the surface of the nano Fe-N alloy powder, gel is formed through drying, and then a SiC layer is coated on the surface of the nano Fe-N alloy powder through high-temperature calcination, so that the wear resistance and mechanical strength of the alloy powder are obviously improved.
Comparative example 5 in comparison with example 3, steps S4 and S5 were not performed. The wear resistance, mechanical property, hardness and thermal conductivity of the alloy are obviously reduced. The tungsten-copper composite material has excellent thermal and electrical properties, higher strength, hardness, low thermal expansion coefficient and better corrosion resistance, a layer of tungsten-copper oxide is deposited on the surface of nano Fe-N alloy powder coated with SiC by a coprecipitation method, and a tungsten-copper alloy material is formed by hydrogen reduction, so that the prepared nano powder alloy material has extremely strong strength, excellent wear resistance, high heat conductivity and high temperature resistance.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (9)
1. The preparation method of the super wear-resistant nano powder alloy material is characterized by comprising the following steps of:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 550-650 deg.c, cooling to room temperature and ball milling to obtain nanometer Fe-N alloy powder;
s2, preparation of Si-C sol: dissolving alkyl orthosilicate and methyl methacrylate in ethanol, adding tert-butyl nitrate at room temperature under the protection of inert gas, stirring and mixing uniformly, adding dilute hydrochloric acid, and stirring until Si-C sol is formed;
s3, preparing SiC-coated nano Fe-N alloy powder: adding the nano Fe-N alloy powder prepared in the step S1 into the Si-C sol prepared in the step S2, uniformly stirring and mixing, drying, calcining, and ball-milling to prepare nano Fe-N alloy powder coated with SiC;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding concentrated nitric acid into a copper nitrate solution to prepare solution A, adding the SiC-coated nano Fe-N alloy powder prepared in the step S3 into an ammonium tungstate solution, carrying out ultrasonic mixing uniformly to prepare suspension B, adding the solution A into the suspension B, stirring to carry out coprecipitation reaction, centrifuging, ball-milling and roasting to prepare the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide and prepared in the step (S4) at 650-750 ℃ for reduction for 2-4 hours to obtain the super wear-resistant nano powder alloy material.
2. The method according to claim 1, wherein powder of at least one of the following is added to the ball mill in step S1: copper powder, nickel powder, chromium powder, zinc powder and graphite powder; the ball milling time is 4-5h, the flow of ammonia gas treatment is 5-7L/min, the content of oxygen in the ammonia gas is 2-3wt% and the content of carbon dioxide is 1-2wt% and the treatment time is 2-3h.
3. The preparation method according to claim 2, wherein graphite powder and nickel powder are added in the ball mill in a mass ratio of 5-7:2.
4. The preparation method according to claim 1, wherein in the step S2, the mass ratio of the alkyl orthosilicate, the methyl methacrylate, the ethanol, the tert-butyl nitrate and the diluted hydrochloric acid is 12-15:2-3:50-70:3-5:15-20, the concentration of the diluted hydrochloric acid is 1-2mol/L, and the time from stirring to forming the Si-C sol is 1-2h.
5. The method according to claim 1, wherein the mass ratio of the nano Fe-N alloy powder to the Si-C sol in step S3 is 5-7:12-15, the drying temperature is 80-90 ℃, the time is 1-2 hours, the calcining temperature is 1200-1300 ℃, the time is 3-5 hours, and the ball milling time is 2-3 hours.
6. The preparation method according to claim 1, wherein in the step S4, the mass ratio of the copper nitrate to the concentrated sulfuric acid is 2-3:10-12, the concentration of the concentrated sulfuric acid is 5.5-6mol/L, the mass ratio of the nano Fe-N alloy powder coated with SiC to the ammonium tungstate is 10-12:3-5, the time of the coprecipitation reaction is 0.5-1h, the roasting temperature is 250-350 ℃, the time is 2-3h, and the time of the ball milling is 1-2h.
7. The method according to claim 1, wherein the aeration amount of the hydrogen gas in step S5 is 13 to 15L/min.
8. The preparation method according to claim 1, characterized by comprising the following steps:
s1, preparing nano Fe-N alloy powder: treating superfine iron powder with ammonia gas at 550-650 ℃ for 2-3h, wherein the flow rate of the ammonia gas is 5-7L/min, the ammonia gas contains 2-3wt% of oxygen and 1-2wt% of carbon dioxide, cooling to room temperature after the reaction is completed, and ball milling for 4-5h to obtain nano Fe-N alloy powder;
adding mixed powder accounting for 5-7wt% of the total mass of the system in ball milling, wherein the mixed powder comprises graphite powder and nickel powder, and the mass ratio is 5-7:2;
s2, preparation of Si-C sol: dissolving 12-15 parts by weight of alkyl orthosilicate and 2-3 parts by weight of methyl methacrylate in 50-70 parts by weight of ethanol, adding 3-5 parts by weight of tert-butyl nitrate at room temperature under the protection of inert gas, stirring and mixing uniformly, adding 15-20 parts by weight of dilute hydrochloric acid, and stirring for 1-2 hours to form Si-C sol;
s3, preparing SiC-coated nano Fe-N alloy powder: adding 5-7 parts by weight of nano Fe-N alloy powder prepared in the step S1 into 12-15 parts by weight of Si-C sol prepared in the step S2, stirring and mixing uniformly, drying at 80-90 ℃ for 1-2h, calcining at 1200-1300 ℃ for 3-5h, and ball milling for 2-3h to prepare nano Fe-N alloy powder coated with SiC;
s4, preparing nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide: adding 2-3 parts by weight of concentrated nitric acid with the concentration of 5.5-6mol/L into 100 parts by weight of aqueous solution containing 10-12 parts by weight of copper nitrate to prepare solution A, adding 10-12 parts by weight of nano Fe-N alloy powder coated with SiC and prepared in the step S3 into 100 parts by weight of aqueous solution containing 3-5 parts by weight of ammonium tungstate, uniformly mixing by ultrasonic waves to prepare suspension B, adding the solution A into the suspension B, stirring to perform coprecipitation reaction for 0.5-1h, centrifuging, ball-milling for 1-2h, and roasting at the temperature of 250-350 ℃ for 2-3h to prepare nano Fe-N alloy powder coated with SiC and deposited with tungsten copper oxide;
s5, preparing a super wear-resistant nano powder alloy material: and (3) introducing hydrogen into the SiC-coated nano Fe-N alloy powder deposited with tungsten copper oxide and prepared in the step (S4) at 650-750 ℃ for reduction for 2-4h, wherein the ventilation amount of the hydrogen is 13-15L/min, and thus the ultra-wear-resistant nano powder alloy material is obtained.
9. A super wear resistant nano powder alloy material prepared by the preparation method of any one of claims 1-8.
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