CN1919515A - Application method of surface alloying ceramic - Google Patents
Application method of surface alloying ceramic Download PDFInfo
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- CN1919515A CN1919515A CN 200610125848 CN200610125848A CN1919515A CN 1919515 A CN1919515 A CN 1919515A CN 200610125848 CN200610125848 CN 200610125848 CN 200610125848 A CN200610125848 A CN 200610125848A CN 1919515 A CN1919515 A CN 1919515A
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Abstract
The invention discloses a ceramic surface modified technology in the composite material preparing domain, which comprises the following steps: designing composite target through the method, alloying the common ceramic surface in the arc furnace to produce composite target with active metal titanium (or zirconium and hafnium) and other needed one or more metal materials (Fe, Ni, Mn, Mo, Cu, Al) according to certain proportion mechanically, evaporating or fusing the composite target acted by arc heat, impact ceramic surface at high speed under high electric field by metal ion.
Description
One, technical field
The application process of surface alloying ceramic of the present invention relates to ceramic surface modification technology and Composite Preparation
Technical field.
Two, background technology
Ceramic material has many advantages, and good etc. as high temperature resistant, corrosion-resistant, high rigidity, wear-resistant and electrical insulating property, therefore, ceramic material has obtained extensive use.But because pottery has inevitable shortcoming,, intensity crisp as property is disperseed and poor processability etc., has limited the further use of pottery.With the ceramic surface alloying, forming surface alloying ceramic is to maximize favourable factors and minimize unfavourable ones to enlarge the main path of ceramic applications.Thereby surface alloying ceramic has broad application prospects.
The greatest difficulty of ceramic surface metallization is because ceramic material is different with the bonding mechanism of metal material, and ceramic material is a covalent bond, and metal material is a metallic bond, so metal is difficult in the ceramic material surfaces wetting and spreading.Therefore also just produced the method for many ceramic surface metallizations, wherein Mn-Mo method and vapour deposition process are the most frequently used methods.The Mn-Mo method is in the sintering process process of complexity, and at ceramic surface, such metallization processes descends ceramic surface fineness with Mn and Mo dusty material sintering, and performance reduces; The characteristics of vapor deposited metal method are that pottery is without undergoing high temperature, can guarantee the dimensional accuracy of part, metalized film is fine and close continuously, thermal conductivity is good, high-frequency loss is little, the intensity height, but only can deposit single metallic element, so can only be called the ceramic surface metallization method, owing to there is not the effect of active element, metal level is lower with the bond strength of pottery in addition.
Advantageous effect based on active element titanium and ceramic chemical reaction, the arc-added glow that applicant was once carried out ceramic surface oozes titanium, but such method only makes ceramic surface realize titaniumization, metallic element is single, conformability is relatively poor, and because the oxyphie ability of titanium is stronger, layer of titanium metal forms oxide-film and is unfavorable for follow-up application process easily by atmospheric oxidn.As being connected of on this basis pottery and metal, because the titanium layer of ceramic surface plating is difficult to all react with solder and mix in brazing process, ceramic side at pottery and metal jointing has kept one deck titanium layer, solder and the wetting of pottery and reaction have been influenced, directly influenced the bonding strength of pottery with metal, the existence of a large amount of intermetallic compound of ceramic side increases joint fragility in the joint, occurs cracking under the residual stress effect easily.
Therefore in order further to enlarge the range of application of pottery, finding out a kind of conveniently surface alloying ceramic preparation method, is imperative.
Three, summary of the invention
The purpose of the application process of surface alloying ceramic of the present invention is to utilize existing conventional ceramic to prepare surface alloying ceramic, conventional ceramic by the present invention designed composition target and process after, make conventional ceramic surface plating one deck contain one or more the alloy-layer with required composition performance in reactive metal titanium, zirconium or hafnium and required metal material iron, chromium, nickel, manganese, molybdenum, copper, aluminium or the silver, surface alloying ceramic has metallicities such as conduction, thermal conductivity on its surface.Further utilize surface alloying ceramic on this basis, realize that pottery is connected with the high-quality soldering of metal.
Surface alloying ceramic, it is characterized in that it being that a kind of composition target that utilizes carries out Alloying Treatment to the conventional ceramic surface in the arc-added glow stove, make conventional ceramic surface plating one deck contain one or more alloy-layer in reactive metal titanium, zirconium or hafnium and required metal material iron, chromium, nickel, manganese, molybdenum, copper, aluminium or the silver, its surface has the surface alloying ceramic of conduction, conductive metal performance.
The preparation method of above-mentioned surface alloying ceramic, it is characterized in that the composition target that utilizes the present invention to design, in the arc-added glow stove, conventional ceramic is carried out surface alloying, composition target evaporates under the effect of arc heat or melts, metal ion under high effect of electric field high-speed impact at ceramic surface, and process spreads and chemical metallurgy reacts plating at ceramic surface, the alloy-layer that the ceramic surface acquisition is made up of these metallic elements, preparation technology parameter is: final vacuum is less than 6Pa, operating air pressure 10～20Pa, the working media argon gas, glow voltage 300～900V, arc current 40～100A, plating time 10～50min, this method can realize the preparation of polytype surface alloying ceramic and laminated composite materials.
The preparation method of above-mentioned surface alloying ceramic, it is characterized in that described composition target is by one or more machinery combinations in proportion in reactive metal titanium, zirconium or hafnium and other required metal material iron, chromium, nickel, manganese, molybdenum, copper, aluminium or the silver, calculate from usable floor area, the shared ratio of Titanium, zirconium or hafnium is 10～40%, and other metallic element proportion is different different because of alloying component respectively.
The application process of a kind of surface alloying ceramic of the present invention is characterized in that it being the pottery behind a kind of surface alloying and the method for attachment of metal, the Si that adopts the surface alloying ceramic preparation method to make
3N
4, ZrO
2, Al
2O
3Or the SiC surface alloying ceramic is connected with xenogenesis pottery behind aluminium foil, carbon steel or the surface alloying, do not need brazing flux, use the Ag-Cu solder, its technological parameter is: final vacuum is less than 6Pa, operating air pressure 10～20Pa, glow voltage 300～900V, 750～900 ℃ of brazing temperatures, temperature retention time 5～15min, working media argon gas, in the arc-added glow stove, realize Si
3N
4, ZrO
2, Al
2O
3Or being connected of SiC surface alloying ceramic and metal, its interface bond strength is greater than 180MPa.
The purpose of preparation surface alloying ceramic is exactly in order to be connected with the metal material soldering, in the selection of composition target, also can consider especially, as select Cu and Ti binary composition target or Ag, Cu and Ti ternary composition target, form Cu-Ti bianry alloy or Ag-Cu-Ti ternary alloy three-partalloy at ceramic surface, these two kinds of materials itself are exactly good solder, thereby help the soldering connection of surface alloying ceramic/metal.So not only save solder, and can carry out soldering to it in (under the atmospheric conditions) under the multiple environmental condition.
Adopt this preparation method also can carry out surface alloying, can form two-sided alloying ceramic the flaky pottery two sides.Also can and weld together, form laminated composite materials two-sided alloying ceramic stack, shown in Figure 5 as accompanying drawing.
This preparation method compares and has the following advantages with existing ceramic metallization method, ceramic/metal method for welding:
1. the metallization and the alloying that help ceramic surface form surface alloying ceramic, have further widened ceramic range of application.
2. avoid single ooze titanium layer obstruction and embrittlement influence, helped alloy-layer and ceramic chemical reaction, improved interface bond strength, reduced the interfacial stress intensity;
3. the composite impregnation-plating alloy-layer is difficult for by atmospheric oxidn.
4. surface alloying ceramic can be under lower vacuum degree condition, even can realize in atmospheric environment that soldering connects; Utilize normal solder to carry out soldering, can obtain good welding point.
5. preparation speed is fast, the efficient height.
Four, description of drawings
Fig. 1 is surface alloying ceramic of the present invention and the used arc-added glow vacuum drying oven of preparation method equipment schematic diagram.1 is cooling circulating water; 2 for plate target be composition target; The 3rd, the furnace wall is the chuck form, inner logical cooling water 1; 4 is additional cathode, plays the heat tracing effect; 5 is the negative electrode pedestal; 6 is seal washer; 7 ceramic workpieces; 8 are the striking hook, are used to light electric arc and pilot arc; 9 is arc power; 10 is the aura power supply.
Fig. 2 is the section of structure of the composition metal target that adopts among surface alloying ceramic of the present invention and the preparation method.
Fig. 3 is the upward view of the composition metal target that adopts among surface alloying ceramic of the present invention and the preparation method.Component difference according to required alloying, material 11,12,13,14 can be in titanium, zirconium or hafnium active element material and iron, copper, nickel, chromium, manganese, aluminium, molybdenum etc. one or more, generally speaking, consider from economic angle, outmost turns is more cheap material, and inner ring is precious materials.For ceramic material, active element is indispensable, because they can carry out certain chemical reaction with pottery.11,12,13,14 material proportions are pressed area and are calculated, because of ceramic material different different and different with required alloy-layer component.
Fig. 4 is a method for welding schematic diagram of the present invention.15 is surface alloying ceramic, and 16 is alloy-layer, and 17 is solder, and 18 is metal (or surface alloying ceramic).Surface alloying ceramic 15, solder 17 and metal 18 are assembled, put into glow soldering stove or vacuum drying oven, the technological parameter according to afore mentioned rules carries out the soldering connection then.
Fig. 5 is the ceramic/metal laminated composite materials.19 is pottery; 20 is metal material;
Five, the specific embodiment
Embodiment 1
Surface alloying Al
2O
3The preparation of pottery, purpose is used for surface conductance.
Pottery is Al
2O
3, composition target adopts titanium, copper, three kinds of components of aluminium, is arranged as copper, aluminium, titanium material from outside to inside, and area ratio is 30～40%, 30～40%, 20～40%.The technological parameter of ceramic surface alloying is:
Final vacuum 6Pa glow voltage 600V
Arc current 60A plating time 30min
The working media argon gas
Al
2O
3The ceramic surface alloy layer thickness is 20 μ m, has excellent conducting performance.
Embodiment 2
Surface alloying ceramic is used for little connection
Ceramic material is Al
2O
3, metal is the aluminium foil behind the 15 μ m, and composition target adopts aluminium, two kinds of compositions of titanium, and employing aluminium is the outer ring, and titanium is an inner ring, the area ratio of aluminium, titanium is 60～80%, 20～40% in the composition target.Surface alloying ceramic is put into vacuum drying oven with metal and solder and is connected.
Ceramic surface alloying and be with the technological parameter of the soldering of metal:
Final vacuum 6Pa operating air pressure 20Pa
Glow voltage 700V arc current 60A
500 ℃ of plating time 50min brazing temperatures
Temperature retention time 10min working media argon gas
Al
2O
3Ceramic surface cemented alloy layer thickness is 10～20 μ m, and the soldering result shows Al
2O
3Ceramic/metal aluminium foil joint flawless, entire joint face is the junction invariably, and the soldered fitting shearing strength is 100MPa.
Embodiment 3
The low vacuum soldering of surface alloying ceramic and metal is used for ceramic/metal and connects
Ceramic material is Si
3N
4, metal material is carbon steel Q235, composition target adopts copper, titanium, three kinds of compositions of iron, employing copper is the outer ring, titanium copper is an inner ring, and the area ratio of copper, titanium, iron is 40～60%, 20～40%, 10～40%, and surface alloying ceramic and metal and Ag-Cu solder are put into vacuum drying oven and carried out soldering.
Ceramic surface alloying and be with the technological parameter of the soldering of metal:
Final vacuum 6Pa operating air pressure 20Pa
Glow voltage 700V arc current 60A
850 ℃ of plating time 50min brazing temperatures
Soldering vacuum 5 * 10
-2Pa temperature retention time 10min
The working media argon gas
The ceramic surface alloy layer thickness is 30 μ m, and the soldered fitting quality is good, Si
3N
4The pottery flawless, entire joint face is the junction invariably, and the soldered fitting shearing strength is 300MPa.
Embodiment 4
Si
3N
4With ZrO
2Low vacuum soldering after the ceramic surface alloying
Pottery is Si
3N
4And ZrO
2, Si
3N
4Composition target adopts copper, titanium, three kinds of elements of nickel during the ceramic surface alloying, and employing copper is the outer ring, and nickel is inner ring, and copper, titanium, nickel ratio are respectively 40～60%, 20～40%, 10～40%, ZrO
2Composition target is selected zirconium, chromium, three kinds of elements of nickel for use during the ceramic surface alloying, and the ratio that zirconium, chromium, nickel account for respectively is 20～40%, 40～60%, 15～30%, and the ceramic solder behind the surface alloying is put into vacuum drying oven and carried out soldering.Its technological parameter is:
Final vacuum 6Pa operating air pressure 20Pa
Glow voltage 800V arc current 60A
930 ℃ of plating time 40min brazing temperatures
Soldering vacuum 0.5Pa temperature retention time 10min
The working media argon gas
The ceramic surface alloy layer thickness is 30 μ m, and soldering is the good joint of obtained performance as a result, Si
3N
4And ZrO
2The ceramic joint flawless, entire joint face is the junction invariably, and the soldered fitting shearing strength is 230MPa.
Embodiment 5
Al
2O
3After the ceramic surface alloying with the arc-added glow soldering of metal
Pottery is Al
2O
3Metal is carbon steel Q235B, and composition target adopts titanium, nickel, three kinds of compositions of aluminium, and the employing titanium is the outer ring, the ratio that titanium, iron, aluminium account for respectively is 20～40%, 20～40%, 30～50%, and pottery after the alloying and metal and solder are put into the aura stove and carried out glow soldering.Ceramic surface alloying and be with the technological parameter of the glow soldering of metal:
Final vacuum 6Pa operating air pressure 20Pa
Glow voltage 600V arc current 60A
900 ℃ of plating time 40min brazing temperatures
Temperature retention time 10min working media argon gas
The ceramic surface alloying layer thickness is about 35 μ m, and soldering is the good joint of obtained performance as a result, Al
2O
3The pottery flawless, entire joint face is the junction invariably, and the soldered fitting shearing strength is 210MPa.
Embodiment 6
ZrO
2After the ceramic surface alloying with metal soldering under atmospheric conditions
Pottery is ZrO
2Metal is carbon steel Q235B, and composition target adopts zirconium, iron, three kinds of compositions of nickel, adopts nickel, is the outer ring, the ratio that zirconium, iron, nickel account for respectively is 20～40%, 40～60%, 15～20%, and pottery behind the surface alloying and metal carry out soldering under atmospheric conditions.Ceramic surface alloying and be with the brazing process parameter of metal:
Final vacuum 6Pa operating air pressure 20Pa
Glow voltage 700V arc current 60A
920 ℃ of plating time 20min brazing temperatures
Temperature retention time 10min working media argon gas
The ceramic surface alloying layer thickness is about 30 μ m, and soldering is the good joint of obtained performance as a result, ZrO
2The pottery flawless, entire joint face is the junction invariably, and the soldered fitting shearing strength is 180MPa.
Embodiment 7
Al
2O
3Ceramic laminated material preparation
Pottery is sheet Al
2O
3, composition target adopts titanium, copper, aluminium, four kinds of compositions of silver, and employing copper is the outer ring, and the ratio that titanium, copper, aluminium, silver account for respectively is 20～40%, 40～60%, 15～20%, 5～10% couples of sheet Al
2O
3Two-sided surface alloying is stacked together 3 two-sided alloying ceramics then, carries out soldering in vacuum drying oven.
Ceramic surface alloying and be with the brazing process parameter of metal:
Final vacuum 6Pa operating air pressure 20Pa
Glow voltage 700V arc current 60A
920 ℃ of plating time 20min brazing temperatures
Temperature retention time 10min working media argon gas
Soldering vacuum 0.5Pa
The ceramic surface alloying layer thickness is that faying face is the junction invariably about 40 μ m.
Claims (1)
1, a kind of application process of surface alloying ceramic is characterized in that it being the pottery behind a kind of surface alloying and the method for attachment of metal, the Si that adopts the surface alloying ceramic preparation method to make
3N
4, ZrO
2, Al
2O
3Or the SiC surface alloying ceramic is connected with xenogenesis pottery behind aluminium foil, carbon steel or the surface alloying, do not need brazing flux, use the Ag-Cu solder, its technological parameter is: final vacuum is less than 6Pa, operating air pressure 10～20Pa, glow voltage 300～900V, 750～900 ℃ of brazing temperatures, temperature retention time 5～15min, working media argon gas, in the arc-added glow stove, realize Si
3N
4, ZrO
2, Al
2O
3Or being connected of SiC surface alloying ceramic and metal, its interface bond strength is greater than 180MPa.
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| JP2000286038A (en) * | 1999-03-31 | 2000-10-13 | Ngk Insulators Ltd | Structure and method for bonding ceramic heater and electrode terminal |
| US6635358B2 (en) * | 2000-07-27 | 2003-10-21 | Ngk Insulators, Ltd. | Composite member comprising bonded different members and method for making the composite member |
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| CN103896635B (en) * | 2014-03-07 | 2015-09-02 | 太原理工大学 | The surface alloying process of powdered ceramic material |
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| CN104973879B (en) * | 2015-07-15 | 2018-05-25 | 哈尔滨工业大学（威海） | A kind of Al2O3The method for sealing of ceramics and ceramic sealing alloy |
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Assignee: Qingyuan elegance Ceramic Co., Ltd. Assignor: Taiyuan University of Technology Contract fulfillment period: 2008.12.15 to 2013.12.15 contract change Contract record no.: 2009440001705 Denomination of invention: Application method of surface alloying ceramic Granted publication date: 20081119 License type: Exclusive license Record date: 20091023 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.12.15 TO 2013.12.15; CHANGE OF CONTRACT Name of requester: QINGYUAN CITY OUYA CERAMICS CO., LTD. Effective date: 20091023 |
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