CN105543939A - Preparation method of particle reinforced compact composite coating layer - Google Patents
Preparation method of particle reinforced compact composite coating layer Download PDFInfo
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- CN105543939A CN105543939A CN201510999544.8A CN201510999544A CN105543939A CN 105543939 A CN105543939 A CN 105543939A CN 201510999544 A CN201510999544 A CN 201510999544A CN 105543939 A CN105543939 A CN 105543939A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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Abstract
The invention discloses a preparation method of a particle reinforced compact composite coating layer. The preparation method is characterized in that diamond powder and carbon powder are mixed for 20-40 h through ball milling according to a ratio of 1: 1-5; the ball-milled mixed powder, anhydrous ethanol and a metal salinized object are mixed to prepare electrophoresis suspension; and the solubility of diamond is 1-5 g/L. A negative electrode material selects a monocrystalline silicon piece; an electrophoresis instrument is electrified to perform electrophoresis deposition for the mixed powder on the monocrystalline silicon piece; and the electrophoresis deposition time is 0.5-5 min. The stirring rotating speed of a magnetic stirrer is 100-500 r/min; when the electrophoresis deposition is finished, a deposition sample is carefully taken out for drying by 18-24 h at a room temperature, is flatly put on the surface of a graphite substrate to put in a high-vacuum reaction furnace, and is heated up to a temperature of 1500-1600 DEG C under inert atmosphere for keeping by 3-10 h; and the composite coating is reactively sintered. The preparation method forms compact silicon carbide combination phases on the surfaces of a basal body and the diamond to improve the bonding strength of the diamond, is uniform and compact in particles of the electrophoresis deposition mixed powder, facilitates full and uniform reaction of the coating layer, and is short in preparation period and low in cost.
Description
Technical field
The present invention relates to a kind of preparation method of compound coating, particularly the preparation method of the fine and close compound coating of a kind of particle reinforce.
Background technology
Diamond has impayable high rigidity and excellent physical and mechanical property, makes diamond tool become the indispensable effective tool of the various stiff materials of processing.Affecting one of principal element of diamond tool work-ing life and performance is that matrix is to adamantine cementability (the plating ability of matrix).Due to diamond and have very high interfacial energy between common metal and alloy, cause diamond particles can not be infiltrated by general low melting point alloy, cementability extreme difference, in traditional manufacturing technology, the mechanical clamping force of diamond particles only by producing after matrix shrinkage is embedded in matrix metal base, and do not form firmly chemical bonded refractory or metallurgical binding, cause that diamond particles is easy to be at work separated with matrix metal base, greatly reduce work-ing life and the performance level of diamond tool.In major part impregnated type instrument, adamantine utilization ratio is lower, and a large amount of expensive diamond comes off at work and runs off among scrap.
Diamond composite has the excellent mechanical property such as high rigidity, high-fracture toughness, high-wearing feature and stable chemical property because of it, gathers around have broad application prospects in industry and military field.Wherein, with diamond, silica flour for precursor powder, utilize silicon carbide-diamond composite that high-temperature high-voltage reaction sintering technology is prepared from, by silicon and the bonding phase of diamond complete reaction Formed SiClx, diamond base material and the bonding matrix material forming atomic scale bonding structure mutually, with be compared with the diamond of bonding phase with cobalt, nickel, not only there is very high hardness and fracture toughness property, and there is higher temperature stability.Silicon carbide in conjunction with phase, because the thermal expansivity of silicon carbide is higher than diamond, because thermal mismatching silicon carbide can produce an appreciable positive stress to diamond, greatly adds matrix to adamantine hold as diamond composite.Silicon carbide is also stiff materials simultaneously, can increase the wear resisting property of matrix material.
Nowadays develop multiple method and prepare diamond based matrix material, comprise block and coating: (1) chemical vapor infiltration (deposition) method (CVI/CVD), a kind of preparation method of gentleness, block materials and coating can be prepared, preparation temperature is lower, material homogeneous is fine and close, can shaping various complicated shape material.But preparation cycle is very long, production cost is high, is difficult to batch production; (2) high temperature brazing method, this method mainly prepares macrobead particle diameter diamond composite coating, the diamond composite coating bonding strength of preparation is high, process cycle is short, but produce very large thermal stresses because metal and diamond thermal expansivity differ greatly, and molten solder metal can in the temperature that can infiltrate to diamond Eroded, induction diamond graphitization.(3) additive method also has electrophoresis-electroplate two step sedimentations, hot spray process, and production cost is low, can produce in batches, but diamond and substrate combinating strength low.Therefore, improving diamond composite over-all properties is the most important thing, and the present invention wishes to prepare diamond composite coating material and further its wear resisting property of raising by electrophoretic deposition in conjunction with silicon infiltration reaction method.
Application number be 201410391801.5 Chinese patent disclose ceramic matric composite and preparation method thereof that a kind of SiC bonds.The ceramic matric composite of described SiC bonding comprises inorganic ceramic base material, polymer infiltration and pyrolysis (PIP)-SiC binding agent, and chemical vapor infiltration (CVI)-SiC binding agent, SiC binding agent is embedded in ceramic base material, and combines closely with ceramic base material.Described inorganic ceramic base material is silicon carbide, silicon nitride, boron nitride, norbide.Preparation method take ceramic powder as base material, Polycarbosilane-xylene solution is binding agent, compression molding prefabricated component, conjugated polymer infiltration pyrolysis method (PIP) and chemical vapor infiltration (CVI) two kinds of methods prepare the ceramic matric composite that high densification SiC bonds.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, aims to provide the preparation method of the fine and close compound coating of a kind of particle reinforce, it is characterized in that, comprise following sequential steps:
I. substrate pretreatment:
(1) monocrystalline silicon piece is put into acetone soln ultrasonic cleaning, then with the acetone that alcohol removing remains, finally use the alcohol that deionized water removing is residual, dry rear for subsequent use, silicon single crystal thickness is 0.1 ~ 1mm;
(2) graphite flake after polished is put into spirituous solution ultrasonic cleaning 10 ~ 15min, re-use the alcohol that deionized water removing is residual, for subsequent use after drying;
Ii. electrophoresis suspensioning liquid preparation:
(1) diamond powder, carbon dust are put into ball grinder in the mixing of 1:1 ~ 5 ratio, after ball milling 5 ~ 10h, form mixed powder;
(2) mixed powder after ball milling, dehydrated alcohol, metal-salt compound are hybridly prepared into electrophoresis suspensioning liquid, wherein diamond solubility is 1 ~ 5g/L;
Iii. aftertreatment:
(1) electrophoresis suspensioning liquid configured is positioned on magnetic stirring apparatus, electrode insertion material, positive electrode material is red copper, stainless steel, nickel, titanium, platinum wherein one are used alone or used in combination, negative electrode material is monocrystalline silicon piece, connect electrophoresis apparatus, start electrophoretic deposition mixed powder on monocrystalline silicon piece, the electrophoretic deposition time is 0.5 ~ 5min.Magnetic stirrer rotating speed is 100 ~ 500r/min;
(2) electrophoretic deposition terminates, and careful taking-up deposited the monocrystalline silicon piece of mixed powder, dries 18 ~ 24h under room temperature;
(3) graphite processed is put into high vacuum Reaktionsofen, the monocrystalline silicon piece depositing mixed powder lies against graphite base surface, rises to 1500 ~ 1600 DEG C of insulation 3 ~ 10h under an inert atmosphere, starts reaction sintering compound coating;
(5), after reaction terminates, silicon carbide-heterogeneous compound coating of silicon-diamond is obtained.
The advantage that the present invention has: 1, form compact silicon carbide in conjunction with phase by metallurgical reaction at matrix and diamond surface, improve adamantine bonding strength; 2, electrophoretic deposition mixed powder uniform particles is fine and close, is beneficial to coating reaction evenly abundant; 3, preparation cycle is short, and cost is low.
Accompanying drawing explanation
Fig. 1 is preparation method's process schematic of the fine and close compound coating of particle reinforce.
10 is diamond particles; 20 is anode electrode; 30 is carbon dust; 40 is monocrystalline silicon piece; 50 is graphite matrix; 60 is silicon carbide-heterogeneous compound coating of silicon-diamond.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
Embodiment 1
I. substrate pretreatment:
(1) monocrystalline silicon piece is put into acetone soln ultrasonic cleaning, then with the acetone that alcohol removing remains, finally use the alcohol that deionized water removing is residual, dry rear for subsequent use, silicon single crystal thickness is 0.1mm;
(2) graphite flake after polished is put into spirituous solution ultrasonic cleaning 10min, re-use the alcohol that deionized water removing is residual, for subsequent use after drying;
Ii. electrophoresis suspensioning liquid preparation
(1) diamond powder, carbon dust are put into ball grinder in the mixing of 1:3 ratio, after ball milling 5h, form mixed powder;
(2) mixed powder after ball milling, dehydrated alcohol, metal-salt compound are hybridly prepared into electrophoresis suspensioning liquid, wherein diamond solubility is 3g/L;
Iii. aftertreatment
(1) electrophoresis suspensioning liquid configured is positioned on magnetic stirring apparatus, electrode insertion material, positive electrode material is red copper, stainless steel, nickel, titanium, platinum wherein one are used alone or used in combination, negative electrode material is monocrystalline silicon piece, connect electrophoresis apparatus, start electrophoretic deposition mixed powder on monocrystalline silicon piece, the electrophoretic deposition time is 1min.Magnetic stirrer rotating speed is 200r/min;
(2) electrophoretic deposition terminates, and careful taking-up deposited the monocrystalline silicon piece of mixed powder, dried 20h under room temperature;
(3) graphite processed is put into high vacuum Reaktionsofen, the monocrystalline silicon piece depositing mixed powder lies against graphite base surface, rises to 1550 DEG C of insulation 5h under an inert atmosphere, starts reaction sintering compound coating;
(5), after reaction terminates, silicon carbide-heterogeneous compound coating of silicon-diamond is obtained.
Embodiment 2
I. substrate pretreatment
(1) monocrystalline silicon piece is put into acetone soln ultrasonic cleaning, then with the acetone that alcohol removing remains, finally use the alcohol that deionized water removing is residual, dry rear for subsequent use, silicon single crystal thickness is 0.3mm;
(2) graphite flake after polished is put into spirituous solution ultrasonic cleaning 12min, re-use the alcohol that deionized water removing is residual, for subsequent use after drying;
Ii. electrophoresis suspensioning liquid preparation
(1) diamond powder, carbon dust are put into ball grinder in the mixing of 1:5 ratio, after ball milling 10h, form mixed powder;
(2) mixed powder after ball milling, dehydrated alcohol, metal-salt compound are hybridly prepared into electrophoresis suspensioning liquid, wherein diamond solubility is 5g/L;
Iii. aftertreatment
(1) electrophoresis suspensioning liquid configured is positioned on magnetic stirring apparatus, electrode insertion material, positive electrode material is red copper, stainless steel, nickel, titanium, platinum wherein one are used alone or used in combination, negative electrode material is monocrystalline silicon piece, connect electrophoresis apparatus, start electrophoretic deposition mixed powder on monocrystalline silicon piece, the electrophoretic deposition time is 3min.Magnetic stirrer rotating speed is 500r/min;
(2) electrophoretic deposition terminates, and careful taking-up deposited the monocrystalline silicon piece of mixed powder, dried 24h under room temperature;
(3) graphite processed is put into high vacuum Reaktionsofen, the monocrystalline silicon piece depositing mixed powder lies against graphite base surface, rises to 1600 DEG C of insulation 10h under an inert atmosphere, starts reaction sintering compound coating;
(5), after reaction terminates, silicon carbide-heterogeneous compound coating of silicon-diamond is obtained.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for the fine and close compound coating of particle reinforce, is characterized in that, comprise following order preparation process:
I. substrate pretreatment
(1) monocrystalline silicon piece is put into acetone soln ultrasonic cleaning, then with the acetone that alcohol removing remains, finally use the alcohol that deionized water removing is residual, dry rear for subsequent use, silicon single crystal thickness is 0.1 ~ 1mm;
(2) graphite flake after polished is put into spirituous solution ultrasonic cleaning 10 ~ 15min, re-use the alcohol that deionized water removing is residual, for subsequent use after drying;
Ii. electrophoresis suspensioning liquid preparation
(1) diamond powder, carbon dust are put into ball grinder in the mixing of 1:1 ~ 5 ratio, after ball milling 5 ~ 10h, form mixed powder;
(2) mixed powder after ball milling, dehydrated alcohol, metal-salt compound are hybridly prepared into electrophoresis suspensioning liquid, wherein diamond solubility is 1 ~ 5g/L;
Iii. aftertreatment
(1) electrophoresis suspensioning liquid configured is positioned on magnetic stirring apparatus, electrode insertion material, positive electrode material is red copper, stainless steel, nickel, titanium, platinum wherein one are used alone or used in combination, negative electrode material is monocrystalline silicon piece, connect electrophoresis apparatus, start electrophoretic deposition mixed powder on monocrystalline silicon piece, the electrophoretic deposition time is 0.5 ~ 5min; Magnetic stirrer rotating speed is 100 ~ 500r/min;
(2) electrophoretic deposition terminates, and careful taking-up deposited the monocrystalline silicon piece of mixed powder, dries 18 ~ 24h under room temperature;
(3) graphite processed is put into high vacuum Reaktionsofen, the monocrystalline silicon piece depositing mixed powder lies against graphite base surface, rises to 1500 ~ 1600 DEG C of insulation 3 ~ 10h under an inert atmosphere, starts reaction sintering compound coating;
(5), after reaction terminates, silicon carbide-heterogeneous compound coating of silicon-diamond is obtained.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107382323A (en) * | 2017-07-24 | 2017-11-24 | 苏州宏久航空防热材料科技有限公司 | A kind of strong silicon carbide filtering membrane preparation method |
| CN112500194A (en) * | 2020-12-13 | 2021-03-16 | 湖南德智新材料有限公司 | Method for forming compact TaC coating on surface of graphite substrate |
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| CN101205625A (en) * | 2006-12-22 | 2008-06-25 | 中国科学院兰州化学物理研究所 | Method for preparing diamond-like composite film containing gold nanoparticles |
| CN101736379A (en) * | 2008-11-22 | 2010-06-16 | 中国科学院兰州化学物理研究所 | Preparation method of super-hydrophilic diamond-like carbon composite film |
| CN102173806A (en) * | 2011-01-24 | 2011-09-07 | 长沙米诺特种陶瓷材料技术有限公司 | Diamond-containing composite material and preparation method thereof |
| CN104674186A (en) * | 2015-02-03 | 2015-06-03 | 上海交通大学 | Method for preparing amorphous silicon carbide ceramic-diamond composite coating |
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| CN101205625A (en) * | 2006-12-22 | 2008-06-25 | 中国科学院兰州化学物理研究所 | Method for preparing diamond-like composite film containing gold nanoparticles |
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| CN107382323A (en) * | 2017-07-24 | 2017-11-24 | 苏州宏久航空防热材料科技有限公司 | A kind of strong silicon carbide filtering membrane preparation method |
| CN107382323B (en) * | 2017-07-24 | 2020-08-25 | 苏州宏久航空防热材料科技有限公司 | Preparation method of strong-bonding silicon carbide filtering membrane |
| CN112500194A (en) * | 2020-12-13 | 2021-03-16 | 湖南德智新材料有限公司 | Method for forming compact TaC coating on surface of graphite substrate |
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