TW386917B - Method of controlling infiltration of complex-shaped ceramic-metal composite articles and the products produced thereby - Google Patents

Description

V. Description of the invention (A7 B7 Central Ministry of Economic Affairs ^ 4,-^ Ά 工 消 消 合作社 卬 卬, the present invention is related to a kind of product that controls the percolation of complex shaped ceramic composite objects and the products made thereby. Typical examples of Tao Wan It is known as a low-density material with high hardness and rigidity; however, it is limited by its nature. It is typically formed by the formation of compacted compacts, due to the large amount of shrinkage that occurs during compaction of compacted compacts. Large and expensive grinding is required to achieve the final shape. Metals are typically non-brittle, non-fragile materials; however, they lack certain desirable properties of ceramics, such as high hardness and rigidity. Therefore, mixed ceramics and metals can be A composite material exhibiting ceramic and metal properties is produced. A method for preparing a ceramic-metal composite object using a ceramic preform is well known to the industry. US Patent No. 5,308,422 discloses a method for preparing a ceramic-metal composite object, which involves forming a ceramic material layer , Sinter the ceramic material layer into a porous ceramic compact, and then immerse the porous body in a molten metal bath to make the porous compact compact into gold Percolation. This method involves uncontrollable metal percolation of the ceramic compaction body, which results in an increase in final cost due to undesired excess metal regions and phases formed on the surface of the composite. Undesired phases occur The reaction phase of the selected ceramic and metal at the diafiltration interface. The reaction phase is chemically unstable, or it will cause coiling damage to the surface of the finished diafiltration product during processing. The coiling damage is caused by the partial removal of non- The desired phase is caused by the undesired phase on the surface of the object, which causes small holes and defects in the surface of the object. What is needed is a complex-shaped ceramic-metal composite object that is prepared after infiltration and requires little or no post-processing. The method is required. The demander is a method to control the infiltration of metal into the ceramic body, so that the metal is in the object ---- ®-(丨 read the precautions on the back before writing the page 4) Order IΦ: • I— II— This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) 5 The central government of the Ministry of Education of the People's Republic of China has 4,-^ d, the consumer cooperation deduction comes from A7 In some areas, the demander is a method for preparing a ceramic-metal composite object, in which an undesired excess metal region and an unwanted phase on the surface are restricted and controlled. The demander is a ceramic-metal composite object, in which Unwanted excess metal areas and unwanted phases on the surface are restricted and controlled. The present invention is a method for preparing a complex-shaped ceramic-metal composite object, which includes: (a) enabling The metal is a non-wet non-wet powder in contact with the molded ceramic body, forming a layer of non-wet powder on one or more surfaces of the molded ceramic body, wherein the molded ceramic object has a region without a non-wet powder layer in between. , And (b) percolating the shaped ceramic body through a region without a non-wet powder layer therebetween, so as to form a complex-shaped ceramic-metal composite including one or more metal phases and one or more ceramic phases, Wherein, the object has a substantially solid shaped ceramic body, an undesired excess metal area on the surface, and a complex-shaped ceramic-metal composite object near the surface. The undesired relationship within is located only in the area without non-wet powder. The invention also relates to a complex-shaped ceramic-metal composite object having an undesired excess metal region and an undesired phase located only on the surface of the object without a non-wet powder layer therebetween. The method of the present invention can prepare a complex-shaped ceramic-metal composite having an undesired excess metal region and an undesired phase located only on the object or on the surface of the object without any non-wettable powder therebetween. The method of the present invention enables the preparation of complex-shaped ceramic-metal composites that require little or no surface adjustment to achieve the final object. A complex-shaped ceramic-metal composite object is prepared, which contains very few undesired excess metal regions and unwanted phases. (Please read the precautions on the back before filling in this page) —, --j installed ------ order ------------

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The central standard of the Ministry of Economic Affairs and only the cooperation and private printing «V. Description of the invention (3) The method of the present invention is used to prepare a ceramic-metal composite object with a complex shape 'which contains one or more metal phases and one or more ceramics phase. The selection of pottery and metal is to enable the metal to wet and percolate the ceramic to form a phase-changing ceramic-metal composite. Furthermore, non-wetting powders have been chosen to avoid unwanted interactions between ceramics and metals. Non-wet powders limit the interface between the metal and the ceramics and prevent or limit the formation of undesired excess surface metals and phases. Therefore, the phase in the coated and reacted ceramic metal system is controlled and desired. The complex-shaped ceramic-metal composite system of the present invention has an object having an undesirably excessive metal area and phase on the surface of an object only in an area without a non-wet powder layer. For example, if the molded article is laminated to a non-wet powder and a small portion of the surface area is not laminated, percolation of the metal may occur through the unlaminated portion. -Once the infiltration has been completed, the unlaminated part of the surface is the only part of the object that contains excessive metal and unwanted phases. This greatly reduces the cost of final processing and surface treatment, because only the unlaminated part needs to be processed, and correspondingly, if traditional filtration technology is used, a large part of the entire surface of the object needs to be processed. Furthermore, a part of the surface of the object may not be laminated, so it contains an undesired metal phantom, but it does not need to be processed, because this part is not necessary for the use of the object. Furthermore, by controlling the area of percolation and excess metal, the formation of unwanted phases can be controlled. By controlling undesired aspects

The stability of the formation phase and the cost of adding T, yfe, a, k iX can be controlled. For example, in an aluminum-metal system with a carbon-containing ceramic, unfiltered and infiltration results in the formation of aluminum carbide on the surface of a swelling object on the side of the aluminum alloy and the surface of the ceramic-metal composite surface and the atmosphere. Wetness in the surface should cause rotten buttons on the surface of the object. This paper is a national standard CNS of the country of wealth) A ^? I72i〇 ^ 97 ^ 7 Φ Install IT (ITPlease read the notes on the back-# 镇 写 页} A7 B7 V. Description of the invention (4) Surface rot button The result is an unrefined coarse sugar surface, which is undesired for most applications. Furthermore, the undesired phase is harder and harder to process smoothly than the desired phase around the surface of the object. Therefore, when processing When it is on the object, the undesired phase on the surface of the object will break away from the surface and cause coiling damage, leaving undesired holes and pits on the surface of the processed object. Therefore, the object cannot be used for the intended purpose. The method of the present invention can be used to prepare any shaped object during which the percolation is desired. Preferably, the method is particularly effective in preparing a complex thin ceramic-metal composite object. A complex-shaped ceramic-metal composite object is preferably Contains at least three phases "Preferred" Each phase is at least 2% by volume based on the volume of the multiphase ceramic metal material. The ceramic-metal composite object preferably has a residual free metal content of 2% by volume or more .Ceramic metal composite The object has a residual free gold content of 75% by volume or less, more preferably 50% by volume or less, and even more preferably 25% by volume or less. The method of the present invention can be used to prepare a ceramic-metal composite object, wherein, The metal penetrates and basically fills the pores of the porous ceramic. Preferably, the ceramic-metal composite object has a theoretical density of 85% or more, more preferably 98% or more, and most preferably 99.5% or more, of which The theoretical density (percentage) is 100 times the ratio of the final measured part density to the theoretical density of the non-porous material. The ceramic-metal composite object is preferably high enough to avoid or reduce bending, sagging during processing and use, The elastic modulus of shaking or resonance. The better one, Tao Jing metal composite object, has confirmed that the elastic modulus is 100 GPa or more, more preferably 150 GPa or more, and more preferably 200 GPa or more. The inventor of the ceramic-metal composite object proves that the flexural strength is high ... The Zhangshang standard universal towel national standard (CNS) M specifications (η to M7 male feet) -8 -----.- Il · Dress ------ ΐτ ------ 0 (Please read the note on the back first Please fill in this page again) A7 B7 Printed by the central government's Ministry of Labor and Consumer Cooperatives f. 5. Description of the invention (Enough to give impact and damage resistance during operation and use. Ceramic modified metal composite object of the present invention Preferably, it is confirmed that the flexural strength is 250Mpa or more, more preferably 350Mpa or more, and more preferably 450Mpa or more. If the conductivity is a desired property, the ceramic-metal composite article of the present invention has a high enough to avoid electrostatic enhancement. Electrical conductivity "Better, if high conductivity is the desired property, the composite object of the present invention has a resistance of 10-2 ohm-cm or less, more preferably 10-4 ohm-cm or less, more It is preferably 10-5 ohm-cm or less. The complex-shaped ceramic-metal composite of the present invention is preferably a computer disk drive assembly. Preferably, the object is a computer hard disk, E-block, actuator, slider, load arm, support arm, actuator bearing, spacer, plywood, mandrel, ball bearing, thrust bearing, base plate, housing or cover set. Even better, these items are E-block actuators and computer hard drives. The metal used in the present invention is selected based on the chemical reaction or wetting ability with the selected ceramic material at elevated temperature, so that the metal can penetrate into the ceramic cavity. Selected metals can be taken from chemical and physical fflwrpr

Press, New York, New York, U.S.A. (1995-1996)) published weekly lists of the newly named Groups 2, 4, 5, 6, 8, 9, 10, 13 and 14, and their alloys. Preferably, the gold used herein includes silicon, magnesium, aluminum, titanium, vanadium, chromium, iron, copper, nickel, cobalt, buttons, tungsten, molybdenum, hammer, niobium, or a mixture thereof and alloys thereof. Aluminum and its alloys are preferred because they exhibit high toughness, good electrical conductivity, and machinability, and they have good wettability with the ceramics used, such as boron carbide. Aluminum is best used as an alloy, which provides improved rigidity over pure aluminum. Aluminum and (: 11,1 ^, 8 丨,: \ 111, (: 1 or one or more of 211 (please read the precautions on the back before filling this page)) The central standard ^^ p industrial consumption cooperation private printing millet A7 B7 5. Invention description (6) alloy is better. Such as eight 1-(^ 11, into 1-1 ^ 1 bar, eight 1-8 丨, eight 1 -1 ^] 1-] ^ 1§ and eight 1- (1: 11-Mg-Cr-Zn alloys and mixtures thereof are more preferred. Examples of these alloys are 6061TM alloy, 7075TM alloy, and 1350TM alloy, which are commercially available Alcoa from Pittsburgh, Pittsburgh. The ceramics used in the present invention were selected based on their chemical reactivity with the selected metal at elevated temperatures in order to increase the penetration of the metal into the ceramic holes. The preferred ceramic used here Contains pendant, gaseous, carbide, gaseous or mixture. Examples of ceramic mixtures include carbide sheds, oxynitrides, oxycarbides and carbonitrides or mixtures thereof. More preferred ceramics are boron carbide, silicon carbide Materials, titanium diboride and boron nitride. The better ceramic material is boron carbide because it has the desired low density and high rigidity, and when compared with the selected Excellent wettability when in contact with metals. Ceramic materials can also be mixed with organic bonding materials (such as paraffin wax, stearic acid or vinylidene, acetate) to facilitate processing. Used to form shaped ceramic bodies The ceramic material is preferably a powder type, typically containing a metal that is chemically bonded to the ceramic with boron, oxygen, carbon, nitrogen, or silicon. The powder ceramic is preferably a crystal with particles of 0.1 micron (0.1 乂 10_3 li) or larger. Material. The powder Taurman is preferably a crystalline material with particles of 50 micrometers (50 × 10 · 3 Li) or smaller, more preferably 10 micrometers (5 × 10-3 mm) or smaller, and even more preferably 5 micrometers (1 × 10). -3mm) or smaller. Crystal particles can be equiaxed, rod-shaped, or small plate-shaped. Examples of preferred ceramic-metal mixtures for forming multi-phase ceramic-metal composite objects include: B4C / A, SiCMJ, TiB2 / A, SiBx / A, SiC / Mg, SiC / Mg, SiC / Mg-A, SiBx / Ti, TiNMJ, TiC / A, ZrB2 / Al, ZrC / A, A1B12 / A, A1B12 / Ti, TiN / Ti, TiC / Ti, TiB2 / B2C / Al The paper size is appropriate / Π China National Standard (CNS) A4 size (210X297 mm) 10 ( Read precautions on the back of reloading the page)

A7 B7 V. Description of the invention (7), SiC / TiB2 / Al, TiC / Mo / Co, ZrC / ZrB2 / Zr, TiB2 / Ni, TiB2 / Cu, TiC / Mo / Ni, SiC / Mo, TiB2 / TiC / A. TiB2 / TiC / Ti, Wc / Co and Wc / Co / Ni. The subscript "X" indicates that the chemicals can have different stoichiometry. More preferred ceramic metal mixtures include: B4C / A, SiCMJ, SiB6 / Al, TiB2 / Al, and SiC / Mg. Most preferably, the material forming the complex-shaped ceramic-metal composite object of the present invention is a chemically reactive system, such as aluminum-boron-carbide. In these chemically reactive systems, the metal components in the percolation can be depleted to form a ceramic phase, which improves properties such as hardness and rigidity. The aluminum-boron-carbide composite material includes at least one boron-carbide phase and at least one aluminum-containing phase. In addition, these phases can be mixed with a filler ceramic. The filler provides the material for the final object, which will not adversely affect the desired properties of the ceramic-metal composite object. The filler may be selected from the group consisting of borides, carbides, nitrides, oxides, silicides, and mixtures thereof. The filler ceramic is preferably used in an amount of 1 to 50% by volume based on the volume of the multi-phase ceramic-based material. The aluminum-boron-carbide composite body preferably includes phases such as B4C, A1B24C4, AUC ^ AlBhAlBmAlBuC ^ AUBwC ^, and free metal A1. The best material is a multi-phase material consisting of B4C, A1 and at least three other ceramic phases, preferably A1B24C4, A13-4BC and A1B2. The B4C particles are preferably surrounded by aluminum boride and aluminum-boron-carbide. In other words, the composite object has a continuous ceramic network formed of aluminum boride, boron carbide, and aluminum-boron-carbide. Non-wettable powders for use in the present invention are selected based on the ability to coat the object and avoid undesired interactions between the selected ceramic and the selected metal. The choice of non-wettable powders depends on the particular ceramic and metal system to be percolated. Non-wettable powder is selected so that the metal can be percolated. This paper is suitable for Chinese National Standard (CNS) A4 size (210x297 feet) 11 (Please read the precautions on the back before filling this page)

V. Description of the invention (8 A7 B7 is printed by the central part of the M section, and only for consumer consumption is used as a social seal? Water and ceramic substrates are non-reactive to the selected metal when used in the substrate and are non-wettable. Money forms undesired excess metal and phases on the surface of the H object. However, when the metal is in contact with some uncoated points on the surface of the substrate, the non-wettable powder cannot prevent diafiltration from occurring in the object. Examples of metal, ceramic, and non-wettable powder systems each include aluminum, boron carbide, and aluminum nitride, and each include aluminum, boron carbide, and aluminum oxide. Preferred non-wettable powder-based nitrides, silicides' oxides, and Mixtures. More preferred non-wettable powders are aluminum nitride, boron nitride, alumina, and mixtures thereof. The most preferred non-wettable powders are aluminum nitride, alumina, and combinations thereof. Preferably, the powder particles may be Can use powder on ceramic body as any size distribution of non-wet powder. The size of non-wettable particles is sufficient to prevent percolation from occurring on the layer of powder particles on the surface on the ceramic substrate. Preferably, non-wet Moist Powder particles have a particle size of ❹ ^ m or larger, more preferably 0.5 microns, and more preferably 1 micron ^ better, non-wettable powders have a particle size of 50 microns or less, more preferably micron or more Less' is more preferably 5 microns or less. The ceramic and metal used in the method of the present invention depends on the desired product. In any embodiment, the selection of ceramic and metal can promote percolation. Percolation is one Method for forming a solid-liquid interface between a metal and a ceramic when the metal is molten, and the metal is a liquid and the ceramic is a solid, and the metal is moved into the hole of the ceramic material by capillary action. Wet contact angle that produces percolation (based on Young equation Definition) The preferred range is less than 90 degrees, the more preferred range is less than 45 degrees, and the optimal range is less than 30 degrees. The method of the present invention includes a series of steps to be performed in order to coat and penetrate the paper. CNS) A4 size (210X297 mm) 12

.II II II I @ 裴 II (please read the notes on the back before filling out this page) -Ding, 119 9 -1¾ The Ministry of Economic Affairs ^ Dong ^ Qiao Gong disappeared in the cooperative 卬 ^-A7 B7 V. Invention Explanation (9) A ceramic-metal composite object having a complex shape containing one or more metals and one or more ceramics is formed by filtering the ceramic body. The preparation of the ceramic body includes forming the selected ceramic into a desired object shape. This step can be performed by various ceramic molding methods described later. The first step of the method involves contacting a selected non-wettable powder with one or more surfaces of the shaped ceramic body. The non-wettable powder may be contacted with the shaped ceramic body by any method in which it is desired to form a non-wettable powder layer on one or more surfaces of the shaped ceramic body without excessive metal deposition. Once the non-wettable powder is in contact with the shaped ceramic body, the next step includes infiltrating the metal into the shaped ceramic body by heating the metal to melt it, wherein the metal selectively penetrates the uncoated holes of the ceramic . The metal percolates through the non-wettable powder during which the molded ceramic body is not laminated on the body. After infiltration, if desired, heat treatment may be performed to impart certain other mechanical properties to the final complex-shaped ceramic-metal composite article. In preparing the ceramic body, the selected ceramic is formed into a final object shape close to the solid body. Any new ceramic molding method can be used, which can form complex shaped parts close to the size of the solid body and close to the shape of the solid body. These ceramic molding methods are well known in the industry, for example, injection molding, slip casting, strip casting, gel casting, pressure slip, DIC pressure, direct processing, extrusion molding, and roll compression. Modern Ceramic Engineering Properties. Processing. And Use in Design, D.W. Richerson and Marcel Pekker, Inc., N.Y, 1982. Preferred ceramic molding methods include injection molding, strip casting, and direct machining. The first step of the method of the present invention includes adapting the non-wettable powder and the shape of the ceramic paper to the Chinese National Standard (CNS) A4 specification (210X297 mm) 13 (Please read the precautions on the back before filling this page). ? τ 5. Description of the invention (1〇) A7 B7 passes through the central part of the M section and only eliminates cooperatives. ^: It is a physical contact in order to form a layer of non-wettable powder on one or more surfaces of the molded Taumann. . Non-wettable powders can be brought into contact with the shaped ceramic body by any method capable of forming a non-wettable powder layer on the formed metal body or surfaces, such as thermal spraying (eg, electric spray spraying), granulation Liquid spraying, dipping clock, spinning, painting, tumble drying, padding, screen (eg, screen printing), sol coating, electrostatic spraying, electrophoretic deposition, scale forming (eg, strip casting), and mixtures thereof . See 'e.g. Elijl £ igl £ s ^ £ reramic p coffee, James Reed, 1988 or u aa, the relevant parts of each document are incorporated herein by reference. The layer may be a layer or the layer may be deposited on the ceramic body in a-pattern. The pattern can be formed by screen printing or masking techniques. More than-non-relevant powders can be used simultaneously. Multi-layer non-wettable powders can also be used. Furthermore, a mixture of a non-wettable powder and an optional metal-wettable powder may be used. Preferably, the non-wettable powder may be mixed with a solvent to form a slurry so as to improve its contact ability with the surface of the shaped ceramic body. It can be done by any conventional technique, such as wet grinding. The non-wettable powder slurry contains a non-wettable powder, a liquid solvent, and optionally one or more binders, plasticizers, and dispersants. Preferred solvents are water, alcohol, and hydrocarbons. Bonding mixtures with various materials. Resins, resins, gums, polyethylene, latex, acrylic acid, lanolin, polypropylene, polystyrene. And other thermoplastic polymers. The plastic can be any plastic that facilitates processing of the slurry mixture. Preferred plastics are glycols, low molecular weight polymers (e.g., liquid at room temperature), oils, fats, and soaps. Dispersant

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-I Description of the invention (11) is any knife powder which can promote knife powder of non-wettable powder and other materials in the slurry mixture. Preferably, in order for the dispersant to function effectively, one wound knife powder needs to be absorbed on the surface of the particles, while the other part is stretched into the solvent J. Strong absorption is caused by the particle surface and the dispersant. Interaction between acid test was achieved. Cationic dispersants (such as amines) are preferably used for negative particle surfaces, while anionic dispersants (such as carboxylic acids) are used for positive particle surfaces. The dispersant used in the present invention is a nonionic dispersant such as ethoxylated nonylphenol, an anionic dispersant such as magnesium stearate, a cationic dispersant such as undecylamine chloride, and amphoteric Dispersants such as dodecyl sweet theophylline. After grinding the non-wet slurry, it is heated, filtered and de-aired to remove air bubbles and agglomerate. The non-wettable paste is in contact with one or more surfaces of the shaped ceramic body. Preferably, the non-wettable powder can be contacted with the shaped ceramic body by dipping, spraying or painting. The spray type includes the use of a sprayer with a spray cabin containing an inert atmosphere or empty milk. After the aforementioned non-wettable powder slurry is sprayed during the spray deposition process, it is uniformly deposited on one or more surfaces of the shaped ceramic body. Spraying consists of controlling the spraying of the slurry and the spraying of the droplets onto the shaped ceramic body or the flow direction on the multiple surfaces. When it collides with the surface of the molded ceramic body, the dripping liquid deforms and condenses into a thick layer. The slurry is dried slowly to avoid cracking of the non-wettable layer and the drying temperature is controlled below the flash point of the selected solvent system. The drying time varies depending on the solvent used and the thickness of the non-wettable powder layer on the shaped ceramic body. It may require the separation of non-wettable powder materials, which can be done by any conventional separation technique, for example, heating in a vacuum or inert atmosphere.

L. Description of the invention (12) The thickness of the layer is generally any thickness that can provide a uniform layer on the surface of the molded ceramic body. In this way, complete contact can be achieved between the non-wettable powder and the selected ceramic. The layer thickness depends on the amount of non-wettable powder and the layer pores. Spraying layer is based on spraying geometry, solid content of slurry, operating distance, spraying time or sequence. Depending on rebound loss and membrane flow. Spraying generally produces a non-wettable powder layer uniformity on the ceramic. The preferred layer thickness is 丨 particle diameter or larger, more preferably 10 particle diameter or larger, and even more preferably 25 particle diameter or larger. A preferred layer thickness is 0.01 or more. A preferred layer thickness is 2 sides or less', more preferably 1 mm or less, and even more preferably 0.25 shirt or less. If desired, the use of screen printing can be used to impart a certain geometry or texture to the non-wettable powder layer on the surface of the shaped ceramic body, thereby further defining the geometry of the composite ^ Printing screens are used in the screens The desired ceramic pattern is formed on the molded ceramic body during printing and the printed pattern is dried. The screen printing method is further described in Screen Priniting I ^ hsiim & ^ _Signs of Times Publishing Co., Cincinnati, Ohio, 19 81 by Kosloff, the relevant part of which is incorporated herein by reference. The next step of the method involves percolating the formed ceramic body with the selected metal 'and thus forming a formed ceramic-metal composite object. Infiltration is a method of forming a solid-liquid interface between metal and ceramics when heated, and the metal is liquid and the ceramics are solid, and the metal moves into the pores of the ceramic material by capillary action. This method preferably forms a completely dense ceramic-metal composite material. Metal percolation in ceramics is produced by a portion of the surface of a shaped ceramic body to which a non-wettable powder is not applied. "Percolation can be performed by any method known in the industry," such as U.S. Patent Nos. 4,702,770 and 4,834,938 No. 2 paper size is deducted from China National Standard (CNS) A4 specification (210X297 mm) II (Please read the notes on the back before filling this page) Set the central standard of the Ministry of Economic Affairs and only eliminate the cooperative deduction System 16 A7 A7 According to the Ministry of Central Standards ^, .jiJ-Consumer Cooperative System ---------------- B7 V. Description of Invention (I3) was merged for reference and permission 4 The method of f materials is adding _, vacuum infiltration, 2 gravity / light heating. When diafiltration is performed, gold: =, which is in contact with the shaped metal body. The wetting angle measured by the t-antenna between metal and Tao Yan can be controlled by selecting the infiltration temperature and time. The temperature of the filter wire depends on the metal used. Percolation is performed at a temperature that can melt the metal but lower than the rapid evaporation of the metal. The preferred temperature for the selection of metal in the selection of Tao Jing depends on the melting temperature of the selected metal. For the inscription 'to make the selected metal penetrate into the selected ceramic, the preferred temperature is i_c or less', more preferably t or less. For example, the preferred temperature for diafiltration in ceramics is 750 ° C or more, and more preferably 900. (: Or greater. For each metal, the correct temperature and time of percolation can be established by determining the contact angle measurement when wetting conditions are reached. Percolation time depends on many factors, such as packing density, Hole radius, void ratio, contact angle, viscosity, surface tension, and sample size. Infiltration is preferably performed until the ceramic material that the metal penetrates is substantially dense. Preferably, it is selected from the metals of the preferred metals and The percolation time between the ceramics selected from the better ceramics is 0.1 hours or more, more preferably 0.5 hours or more, and more preferably 丨 hours or more. The percolation time with the pottery tin selected from the better ceramics is 24 hours or less, more preferably 12 hours or less, and more preferably 6 hours or less. The preferred time in the carbonized shed (at 1100 ° C) is 10 minutes. Diafiltration can be completed at atmospheric, negative or superatmospheric pressure. Diafiltration is preferably performed under an inert gas (such as' argon or nitrogen) or under vacuum Implementation. At superatmospheric pressure, the temperature of the paper Zhang scale is applicable to Chinese National Standard (CNS) A4 specification (210X297 mm) 17 (Please read the precautions on the back and save and fill in this education) Order-.

V. Description of the invention (I4) According to the central standard of the Ministry of Civil Affairs, the labor force can be reduced. Infiltration is preferably performed until the ceramic-metal composite is densified to a density greater than 85%, more preferably greater than 98% of the theoretical density, and most preferably greater than 99.5% of the theoretical density. Once the infiltration step is completed, a complex-shaped ceramic-metal composite object with complete infiltration is formed. After the infiltration, a heat treatment can be selectively applied to the ceramic-metal composite part to further define the mechanical properties of the object. A preferred method of altering the microstructure of a ceramic composite that has been infiltrated involves post-diafiltration to heat the previously infiltrated composite. Mechanical properties that can be specified include fracture toughness, fracture strength, and hardness. This additional step of heating the ceramic-metal composite object at a selected temperature for a selected time will reduce the amount of residual free metal and improve the homogeneity of the multi-phase ceramic material. As a result of the post-diafiltration heat treatment, the slow growth of the ceramic actually occurs. The formation of polyphases in ceramic-metal composites and the maximum control of the above mechanical properties are achieved during heat treatment. The temperature at which the heat treatment is performed is the temperature at which the residual free metal is reduced. Furthermore, the temperature at which the heat treatment is performed is the lowest temperature at which a solid-state chemical reaction occurs. A preferred method of altering the microstructure of a ceramic metal composite that has been infiltrated includes post-heat treating the composite that has been infiltrated at 65 ° C or greater, more preferably 700 ° C or greater. The maximum temperature of the post-heat treatment is the melting point of the metal in the ceramic-metal composite object. The heat treatment time is preferably long enough to achieve the desired properties in the ceramic-metal composite object by changing the microstructure. For example, in the case of aluminum-boron-carbide, this additional heat treatment step is preferably completed by heating the percolate to a temperature of 60 ° C or more, more preferably 700t or more, More preferably, it is 80 ore or more. More preferably, the heat treatment is performed at a temperature of 1500 ° C or lower, and more preferably 1200 β (: or

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—.1 IIIIII, invention description (is) is lower, more preferably 100 (TC or lower. The preferred time for heat-treating aluminum-boron-carbide is 1 hour or more, and more preferably 25 hours or more. The heat treatment may be performed in air or an inert atmosphere, such as nitrogen or argon. Preferably, the heat treatment is performed in the air. After percolation and selective heat treatment, the percolate is cooled. Alternatively, the percolate may be By mechanical polishing to the final desired shape. Undesirable excess metal on the surface not treated with non-wettable powder can be removed by mechanical polishing. Depending on the final use of the percolation object, it may be desired to polish the percolation object For example, if the desired object is a computer hard disk, the surface of the disc needs to be polished to a substantially uniform average roughness value between 1 and 2000 A. After the infiltration or selective heat treatment step, the non-wettable powder can be removed from the object. The surface can be removed. The removal of non-wettable powder can be performed by any method known to those skilled in the art. Examples of removal methods include ultrasonic treatment or mechanical washing in water or other solvents. Preferred ,shift The method is based on sonication in water. Furthermore, for example, if the desired object is a computer disk drive, coating can be applied to the disk drive to impart surface texture to the composite object. Suitable coatings are, for example, nickel-phosphorus coatings However, other types of coatings can be used, such as metals and polymers. If nickel-phosphorus coatings are used on objects, such as computer hard disks, today's industries can be used to prepare and use magnetic disks. Procedure. The coating method can be any method that provides dense coating, such as atomic deposition, particle deposition, monolithic coating or surface modification. The most typical coating method is electroplating, and the coating itself can be further processed to the whole Provide a textured surface on the surface or a part of the surface. Further processing can be performed by, for example, mechanical technology, chemical

V. Description of the Invention (16) The " * Ministry Central Samples " is completed only by consumer, consumer, printing, or optical technology, electrical technology, or a combination thereof. In a preferred embodiment of the present invention, the ceramic tape ( For example, carbonized sheds) are first cast into strips. In the casting belt, at least one ceramic molded body is formed by removing a part of the tape using a technique such as impact, which remains behind the molded body of the casting belt. The ceramic molded body is attached to the tape by one or more thin elements also formed in the tape. These thin elements serve as conductors of the metal percolated into the molded body, and these elements can be mechanically broken after permeating the tape with metal. Prior to percolating a casting band with a shaped ceramic body in between, the band is generally separated as described herein, and then a non-wet powder (e.g., AIN is applied) (e.g., spraying) is left on the band. The next tape of the ceramic molded body in the area not in contact with the non-wet powder. Then, the tape was percolated as described above. After infiltration, it has been infiltrated; considered ceramic shapes (ie, complex-shaped ceramic-metal composites) are removed from the infiltration belt, for example, by breaking a thin element and removing the composite And do it. After the composite is removed, it can be post-treated 'e.g.' as previously described to remove the non-wet powder and then ground to the final shape. The method for preparing a complex-shaped ceramic-metal composite object can be generated from a complex-shaped ceramic-metal composite object with little or no unexpected excess metal on the outer surface of the object after percolation. Controlled infiltration and the expectation that near-solid objects can be formed by this method "The preferred product of the present invention is a computer hard disk starting element, in which the material has high hardness, high wear resistance, high fracture toughness, high Damping capacity, low density, high specific rigidity, and conductivity. For ceramic-metal composite objects with complex shapes, there are other applications, such as pressure boxes, automotive paper standards, universal China-National Standard (CNS) six 4 specifications (210 > < 297 publicly available > '----- (Please first Read the notes on the back and fill out this page) @ 装 ；

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After "quotation", only the engine parts, brake systems or any parts that need to be infiltrated. The following examples are for illustrative purposes only and are not intended to limit the scope of patent applications in this case. Example 1 Raw parts of carbonized collar (B4C) were prepared by mixing 3284 g of ESKF1500B4C powder and 114.78 g of organic binder, plasticizer and dispersant. These components were mixed at 60 rpm / 130 eC in a 260 ml bowl attached to a HaakeRhecosystem System 40 Torque Rheometer to form a mixture having a solid volume content of 50.1%. The composition was injection-molded into a shape occupying approximately 9.1 cm3, which was at a barrel temperature of 93.3 and an injection rate of approximately 600 cm3 / sec. The part is detached according to the following approximate heating method. 〇 / hour-310 ° C, 10. (: / Hour one 375. (:, 20. (: / hour one 430. (:, 7 CM, hour 500 ° C, 30 ° C / hour one 530 ° C, and use an oxide in a nitrogen atmosphere ( AlcoaA-16SG) The powder bed was cooled to room temperature. The parts were spray-coated and dried with a mixture of 10v / o aluminum nitride / 90v / o ethanol (mixing ratio of 360ml ethanol / 128g AIN). The bottom surface remained Spray. Approximately 15.2 grams of 6061TM aluminum alloy plate is placed in contact with the uncoated bottom surface of the part. The part is then placed on a Saffil bed and diafiltered in an AVS furnace under vacuum at 1160 ° C for 2 hours and It is rapidly cooled through the furnace water jacket. The formed part has excess surface aluminum only at the bottom of the part (without non-wettable powder placed in between). Example 2 Raw parts are molded as in Example 1. The parts are made in ethanol and Al2〇3 (non-wet for aluminum) slurry mixture (20.6v / 0 Alcoa A-16 This paper size is suitable for China National Standards (CNS) A4 size (210X297 mm) -21-(Please read the back first Please pay attention to the refill this page j Φ Pack--Order-A7 B7 Central sample rate of the Ministry of Economic Affairs and UJ Consumer Cooperative printing _ 386917 '—1 —---------- V. Description of the invention (I8) Sg (ultra-abrasive), 79.4v / ο ethanol) immersion; the bottom surface was wiped clean to provide a starting point Percolate the surface and allow it to dry in the air. Then place the part in an oxidized bed (Alcoa A-16 Sg) and use it as a capillary aid during detachment. The following heating methods are implemented: 7. (: / hour -10. (:, 5 ° C / hour-310 ° C, 10 ° C / hour-375 ° C, 20 ° C / hour-410 ° C, 7 ° C / hour-500 ° C, 30 ° C / Hour_ 540 ° C, and cooled to room temperature in a nitrogen atmosphere. After the separation step, the coating is still attached to the surface of the part, so that the sample can be used directly in the conditions of diafiltration as described in Example 1. Example 3 100 parts by weight of boron carbide powder (having an average particle size of 1 to 1.5 microns; available from Elektroschmelzwerk kempten, Germany) and 22 parts by weight of methyl ethyl ketone and 14 parts by weight of isobutyl methacrylate adhesive (available from Rohm & Haas Company, PA) and 6 parts by weight of dibutyl uric acid ester (available from Aldrich Chemical Company) are mixed to form a slurry of boron carbide powder. 1 added carbon Shed powder material is filled in 2 extra (8 liter) acrylic bottles (the 1/3 of which is filled with 5/8 inch pair (16mm) diameter and 5/8 inch leaf (16mm) hot dust carbonized cylindrical cylindrical grinding medium. Mill in balls for 12 to 16 hours. After grinding, the slurry had a viscosity of 3000 cp (the shear rate at 5 sec-1 was measured with a Haake VT-500 viscometer). An 18-inch (457.2mm) wide band is cast from a slurry on polyester (MYLARTM, available from Dupont de Nemours, Wilmington, DE) film (coated with a silicone release agent to form a casting strip. The solvent (ie , Methyl ethyl ketone) is formed from the casting belt by drying in the air at room temperature to form a drying belt with a thickness of 0.6 sides. Use a knife to remove part of the drying belt, and the drying belt is buckled according to the Chinese National Standard (CMS) A4 specification ( 210X297 mm> 22 (Please read the precautions on the back before filling in this page) 'Installation-, · §! 386917 A7 B7 V. Description of the invention (i9) Cut to form a flat triangle in the belt, which is obtained by At the angle between the first thin element extending from the middle of one side of the triangle and the second thin it attached to the side of the first thin element, it is attached to the rest of the drying belt. The side of the triangular body is 6 cm long .Thin components are 0.9 coffee wide and 0.14 coffee long. The adhesive and plasticizer are heated at 100 ° c / hour for 6 hours to 450 C, and maintained at 450 C for 60 minutes (under flowing nitrogen), and then 5.0 ° / min Cool to room temperature, and dry from ceramic molding The tape was removed. The strip was placed in a flat alumina shaper, and then the upper side of the tape was sprayed with a mixture of 10v / 0 aluminum nitride / 90v / o ethanol until the tape was covered with AIN powder. The small area of the edge of the belt is separated from the ceramic molded body of the belt. An aluminum 606i alloy sufficient to permeate the entire release belt is placed in the uncoated area of the release belt. The shaper, the belt and the aluminum flow in the furnace. It was heated to 1100 C under argon and kept at 1 100 ° C. for 4 hours. After cooling to room temperature, the beads were struck with glass beads under the diafiltration belt to remove the ALN powder and the diafiltration ceramic molded body (ie, molding The ceramic-metal composite) is removed by breaking the thin element (during which it meets the rest of the percolation belt). Remove the ceramic-metal composite on the percolation belt with 9mni sides to leave a square hole. (Please Read the notes on the back before filling this page), va Γ d Central Standards of the Ministry of Economic Affairs, and only printed by consumer cooperatives 23 This paper size applies to China National Standard (CNS) A4 (210X297 mm)

Claims (1)

Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs §86917! 8s ___ D8 VI. Patent application method A method for preparing a complex-shaped ceramic-metal composite object, comprising: (a) making the non-wetted non-wet powder and The shaped ceramic body contacts to form a layer of non-wet powder on one or more surfaces of the shaped ceramic body, wherein the shaped ceramic object has a region without a non-wet powder layer therebetween, and (b) the shaped ceramic body is passed therethrough The area without the non-wet powder layer is percolated with the metal, so that a complex-shaped ceramic-metal composite including one or more metal phases and one or more ceramic phases is formed, wherein the object substantially has a nearly solid shaped ceramic body, and Unwanted excess metal areas on the surface and complex-shaped ceramic-metal composite objects close to the surface are located only in areas where there are no non-wet powders. 2. The method of claim 1 in the scope of patent application, the ceramic of which is applied to the shaped ceramic body is boride, oxide, carbide, nitride, silicide or mixture thereof β 3, as in the scope of claim 2 of patent application In this method, the ceramic is a boron carbide or a silicon carbide. 4. The method of claim 3 in the scope of patent application, wherein the metal is Shi Xi, Zhen, Lu Ti Heng, Chromium, Iron, Steel, Lu, Ming, Group, Crane, Turner, Niobium, or a mixture thereof. 5. The method according to item 4 of the patent application, wherein the metal is an inscription and the ceramic is a side carbide. As stated in the method of patent scope item 5, wherein the non-wettable powder is 24 ί88 』Patent application scope ϊ a nitride, oxide or petrochemical or mixture thereof. 7 'Method of enumerating item 6', wherein the non-wettable powder is a nitride, an oxide, boron nitride, or a mixture thereof. 8. The method of claim 7 in the scope of patent application, wherein the metal is an inscription, the ceramic is boron-carbide, and the non-wettable powder is aluminum nitride. For example, the method of item 8 of the patent is stated, wherein the shaped ceramic body is formed by injection molding, slip casting, strip casting, gel casting, pressure slip casting, DIC pressure, direct processing machinery, and extrusion. Or formed by rolling and shrinking. 10. The method according to item 9 of Shenqing Patent Ia, wherein the non-corrosive powder is contacted with the shaped ceramic body by dipping, spraying or painting. 11. The method of item 1 of the patent application park, which brings the non-wettable powder and powder wettable to the metal into contact with different parts of the surface of the shaped ceramic body. For example, the method of claim 9 of the scope of patent application, the molded ceramic body is formed by strip casting and then removing a part of the casting belt to form a molded body on the casting belt. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 13. If the method of the scope of patent application is No. 12, wherein the infiltration is applied to the belt having the molded ceramic body therein, the molded ceramic-metal composite is self-ceding infiltration belt Remove it. 14. A complex-shaped ceramic-metal composite article which can be obtained by the method of patent application Nos. 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, or 13. 15. If the object of the scope of patent application is item 14, the object is a computer hard disk, E-block, actuator, slider, load arm, support arm, moving shaft. The paper dimensions are applicable to Chinese National Standards (CNS). A4 specification (210X297 mm) 25 A8 386917 I 6. Application scope of patent, spacer, cool plate, mandrel, ball bearing, thrust bearing, base plate, housing or cover sleeve. 16. The article of claim 15 in which the article is an E-block actuator or a computer hard drive. ----- 卜 i 转 ------ 定 ------ #. (Please read the precautions on the back before filling out this page) Printed on this paper. Applicable to the standard printed by the Staff Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. China National Standard (CNS) A4 Specification < 210X297 mm) 26