CN1325431C - Gel molding-injection base from high-strength ceramic composite materials and shaping method thereof - Google Patents
Gel molding-injection base from high-strength ceramic composite materials and shaping method thereof Download PDFInfo
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- CN1325431C CN1325431C CNB2005100449204A CN200510044920A CN1325431C CN 1325431 C CN1325431 C CN 1325431C CN B2005100449204 A CNB2005100449204 A CN B2005100449204A CN 200510044920 A CN200510044920 A CN 200510044920A CN 1325431 C CN1325431 C CN 1325431C
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Abstract
The present invention discloses a gel injection molding base substrate made from high strength ceramic composite material and a forming method thereof, which comprises an organic monomer which takes up less than 5 % of the weight of the base substrate, a cross-linking agent, a dispersing agent, an initiating agent, a catalytic agent and ceramic composite powder which takes up more than 55% of the volume of the base substrate, wherein the composite powder is composed of an iron aluminum intermetallic compound and aluminum oxide, the weight ratio of which is (10 to 30): (90 to 70). The key to the gel injection molding technology of the present invention lies in that the composite powder is dispersed in a solution which comprises the organic monomer and the cross-linking agent. Ceramic slurry which forms high solid phase volume fraction is injected in a formed mould. Composite powder concentrated slurry with high solid volume content which is more than 55% and low viscosity which is less than 1000MPa. s is obtained because of the function of the dispersing agent, the initiating agent and the catalytic agent, and the organic polymerization reaction of the slurry occurs under the temperature of 60 to 80 DEG C. Ceramic composite material products with complex shape, large size and high accuracy are obtained after solidifying forming, dryness, degreasing and sintering.
Description
Technical field
The present invention relates to the improvement of ceramic composite, particularly high-strength ceramic composite materials gel injection moulding blank and forming method thereof, i.e. the gel casting forming technology of intermetallic compound/alumina ceramic composite material.It belongs to the synthetic preparing technical field of inorganic materials
Background technology
In the preparation process of high-performance ceramics, the forming method of employing mainly is divided into dry method and wet method two big classes at present.In order to widen the range of application of stupalith, practical application requires ceramic product is prepared into various complicated shapes more and more, and wet moulding can both reach this purpose greatly.But all there are some problems in traditional wet moulding technology, is to absorb moisture by plaster mold to realize as injection forming, causes the blank density distribution gradient easily, shrink when dry inconsistent, product easy deformation, and blank strength is low, is easy to damage.Hot die-casting molding or injection molding need add wax or the organic polymer about 20% (massfraction), cause subsequently de-waxing or degreasing difficulty, and in the process of de-waxing or degreasing, cause blank strength to reduce, easily produce defective even collapse, therefore also be not suitable for preparing complicated shape, large-sized goods.
Gel-casting method (gelcasting) has overcome injection forming, hot die-casting molding and injection molding most shortcoming, be particularly suitable for preparing complicated shape, large-sized ceramic, and have plurality of advantages such as reliability height, good product quality, production cost be low.This method combines traditional ceramic grout forming technique and polymer chemistry theory well.The used organism of gel casting forming is few, and degreasing is easy, and the blank strength height, can carry out machining, thereby has more wide application prospect.At present, gel casting forming is used for the preparation of pure ceramic product mostly, does not see to be used to prepare intermetallic compound-ceramic composite.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provides a kind of new high-strength ceramic composite materials gel injection moulding blank and forming method thereof, i.e. the moulding new technology of intermetallic Fe-Al compound/alumina ceramic composite material.
The objective of the invention is to realize that by following technical scheme developed a kind of high-strength ceramic composite materials gel injection moulding blank, it comprises: account for the organic monomer below 5% of described green body quality, linking agent, dispersion agent, initiator and catalyzer; Also comprise the ceramic composite powder more than 55% that accounts for described base substrate volume.Described ceramic composite powder is made up of intermetallic Fe-Al compound and aluminum oxide, and wherein the mass ratio between intermetallic Fe-Al compound and the aluminum oxide is (10-30): (90-70), the mean particle size of this ceramic composite powder is at 1～10 μ m.
Described ceramic composite powder, it still is to be made up of Intermatallic Ti-Al compound and aluminum oxide, and wherein the mass ratio between Intermatallic Ti-Al compound and the aluminum oxide is (5-30): (95-70).
Described ceramic composite powder, it still is to be made up of intermetallic Ni-Al compound and aluminum oxide, and wherein the mass ratio between intermetallic Ni-Al compound and the aluminum oxide is (5-40): (95-60).
A kind of forming method of described high-strength ceramic composite materials gel injection moulding blank.Described method steps is as follows:
(1) preparation premixed liquid: add organic monomer and linking agent in the deionized water of constant volume, the mass percent that forms premixed liquid is 18～35%, and the mass ratio between this organic monomer and the linking agent is (10～120): 1;
(2) add ceramic composite powder: add ceramic composite powder in (1) step premixed liquid, the add-on of this composite granule is (40～80) in its volume and premixed liquid volume ratio: the ratio of (60～20) adds, and makes slurry;
(3) add dispersion agent: in (2) step slurry, add 3～8% dispersion agent;
(4) regulate the pH value: regulate (3) step pH value of slurry 8～11 with ammoniacal liquor;
(5) ball milling slurry: (4) are gone on foot prepared slurry ball milling 8～12 hours, obtain solid volume content＞55%, and the composite granule underflow material of viscosity＜1000mPas;
(6) add initiator and catalyzer: (5) step slurry temperature is remained between 0～40 ℃, the initiator of adding 0.01～2% and 0～2% catalyzer, after stirring, again with this slurry through the vacuum stirring de-bubble, make ceramic size;
(7) injection forming: in (6) step ceramic size injection moulding mould, and under 60～80 ℃ temperature, be molding blank with the ceramic slurry curing in the mould;
(8) drying forming base substrate: the molding blank after will solidifying promptly gets gel injection moulding blank 50～80 ℃ of oven dry down; Dry later gel injection moulding blank and can also carry out machining according to the specific requirement of product.
(9) base substrate after the machining is placed the kiln degreasing, and after degreasing, then carry out sintering and make combined ceramic products.
Described organic monomer is acrylamide (AM), or Methacrylamide, or oxyethane.
Described linking agent is N, N '-methylene-bisacrylamide (MBAM), or the ethylene glycol that cooperates with oxyethane.
Described dispersion agent is the ammonia soln of polymethyl acrylic acid (PMAA), or polyacrylic ammonia soln, or the polyacrylic acid sodium water solution.
Described initiator is an ammonium persulfate aqueous solution, or superoxol.
Described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMDE).
Beneficial effect of the present invention is: owing to selected to account for the ceramic composite powder of being made up of intermetallic Fe-Al compound and aluminum oxide more than 55% of described base substrate volume.Contain Fe in this intermetallic Fe-Al compound
3Two kinds of compounds of Al and FeAl; Its powder preparing adopts mechanical alloying to add 1 hour technology of 750 ℃ of calcinings.Mass ratio in this ceramic composite powder between intermetallic Fe-Al compound and the aluminum oxide is (10-30): (90-70).Or account for the ceramic composite powder of forming by Intermatallic Ti-Al compound and aluminum oxide more than 55% of described base substrate volume; Mass ratio in this ceramic composite powder between Intermatallic Ti-Al compound and the aluminum oxide is (5-30): (95-70).Or account for the ceramic composite powder of forming by intermetallic Ni-Al compound and aluminum oxide more than 55% of described base substrate volume; Mass ratio in this ceramic composite powder between intermetallic Ni-Al compound and the aluminum oxide is (5-40): (95-60).The granularity of all ceramic composite powders is at 1～10 μ m.These ceramic composite powders are scattered in and contain organic monomer: acrylamide (AM), or Methacrylamide, or oxyethane, and linking agent: N, N '-methylene-bisacrylamide (MBAM), or in the solution of the ethylene glycol that cooperates with oxyethane, constituted the suspensoid of high solid volume fraction.This suspensoid is in mould, and the netted polymerization of macromolecular original position combines the composite granule particle, so that organic monomer solution becomes the low-viscosity carrier of undertaking composite granule, again by the effect of linking agent, makes slurry form the gel of polymkeric substance.Owing in slurry, add 3～8% polymethyl acrylic acid ammonia (PMAA) as dispersion agent; Regulate pH value of slurry 8～11 with ammoniacal liquor; With prepared slurry ball milling 8～40 hours, add slurry temperature is remained between 0～40 ℃, the initiator of adding 0.01～2% and 0～2% catalyzer, after stirring, again with this slurry through the vacuum stirring de-bubble, obtained high solid volume content＞55%, and the composite granule underflow material of low viscosity＜1000mPas; These all are the keys of gel injection technology.
Embodiment
Embodiment
Add the organic monomer and the linking agent of 20% (wt) in deionized water, the proportioning of organic monomer and linking agent is 24: 1, makes premixed liquid; With median size is that the alpha-aluminium oxide powder of intermetallic Fe-Al compound powder about 2 μ m and same particle size mixes and makes composite granule, the intermetallic Fe-Al compound powder accounts for 10%～30% of whole powder quality, join and make slurry in the premixed liquid, the volume fraction of composite granule is 55% in the slurry; Add concentration and be the ammonia soln 3% of 5% polymethyl acrylic acid in slurry, regulating pH value of slurry with ammoniacal liquor is about 10, ball milling 12 hours; Treat slurry temperature below 40 ℃ the time, add concentration and be 5% ammonium persulfate aqueous solution 0.1%, continued ball milling 10 minutes; Pour out slurry from ball mill, put into vacuum chamber and vacuumize degasification, vacuum tightness is 400mmHg, keeps 2 minutes; From vacuum chamber, take out slurry, in the injection moulding mould, put into 80 ℃ water-bath curing molding.Demoulding after drying, degreasing are burnt till at 1550～1650 ℃ again, are incubated 1 hour.Obtain fine and close intermetallic Fe-Al compound/alumina ceramic composite material goods at last.Other prescription and the main technique condition of the formed material of gel injection moulding blank see Table 1.
Table 1:
Those of ordinary skill in the art can understand, and in protection scope of the present invention, makes amendment for the foregoing description, and it all is possible adding and replacing, and it does not all exceed protection scope of the present invention.
Claims (9)
1, a kind of high-strength ceramic composite materials gel injection moulding blank, by the organic monomer below 5% that accounts for described green body quality, linking agent, dispersion agent, initiator and catalyzer and the ceramic composite powder more than 55% that accounts for described base substrate volume are made, it is characterized in that: described ceramic composite powder is made up of intermetallic Fe-Al compound and aluminum oxide, wherein the mass ratio between intermetallic Fe-Al compound and the aluminum oxide is (10-30): (90-70), the mean particle size of this ceramic composite powder is at 1～10 μ m.
2, a kind of high-strength ceramic composite materials gel injection moulding blank, by the organic monomer below 5% that accounts for described green body quality, linking agent, dispersion agent, initiator and catalyzer and the ceramic composite powder more than 55% that accounts for described base substrate volume are made, it is characterized in that: described ceramic composite powder, it still is made up of Intermatallic Ti-Al compound and aluminum oxide, wherein the mass ratio between Intermatallic Ti-Al compound and the aluminum oxide is (5-30): (95-70), the mean particle size of this ceramic composite powder is at 1～10 μ m.
3, a kind of high-strength ceramic composite materials gel injection moulding blank, by the organic monomer below 5% that accounts for described green body quality, linking agent, dispersion agent, initiator and catalyzer and the ceramic composite powder more than 55% that accounts for described base substrate volume are made, it is characterized in that: described ceramic composite powder, it still is made up of intermetallic Ni-Al compound and aluminum oxide, wherein the mass ratio between intermetallic Ni-Al compound and the aluminum oxide is (5-40): (95-60), the mean particle size of this ceramic composite powder is at 1～10 μ m.
4, a kind of forming method as high-strength ceramic composite materials gel injection moulding blank as described in claim 1 or 2 or 3, it is characterized in that: described method steps is as follows:
(1) preparation premixed liquid: add organic monomer and linking agent in the deionized water of constant volume, the mass percent that forms premixed liquid is 18～35%, and the mass ratio between this organic monomer and the linking agent is (10～120): 1;
(2) add ceramic composite powder: add ceramic composite powder in (1) step premixed liquid, the add-on of this composite granule is (40～80) in its volume and premixed liquid volume ratio: the ratio of (60～20) adds, and makes slurry;
(3) add dispersion agent: in (2) step slurry, add 3～8% dispersion agent;
(4) regulate the pH value: regulate (3) step pH value of slurry 8～11 with ammoniacal liquor;
(5) ball milling slurry: (4) are gone on foot prepared slurry ball milling 8～12 hours, obtain solid volume content＞55%, and the composite granule underflow material of viscosity＜1000mPas;
(6) add initiator and catalyzer: (5) step slurry temperature is remained between 0～40 ℃, the initiator of adding 0.01～2% and 0～2% catalyzer, after stirring, again with this slurry through the vacuum stirring de-bubble, make ceramic size;
(7) injection forming: in (6) step ceramic size injection moulding mould, and under 60～80 ℃ temperature, be molding blank with the ceramic slurry curing in the mould;
(8) drying forming base substrate: the molding blank after will solidifying promptly gets gel injection moulding blank 50～80 ℃ of oven dry down.
5, according to the forming method of the described high-strength ceramic composite materials gel injection moulding blank of claim 4, it is characterized in that: described organic monomer is an acrylamide, or Methacrylamide, or oxyethane.
6, according to the forming method of the described high-strength ceramic composite materials gel injection moulding blank of claim 4, it is characterized in that: described linking agent is N, N '-methylene-bisacrylamide, or the ethylene glycol that cooperates with oxyethane.
7, according to the forming method of the described high-strength ceramic composite materials gel injection moulding blank of claim 4, it is characterized in that: described dispersion agent is the ammonia soln of polymethyl acrylic acid, or the ammonia soln of poly amic acid, or the polyacrylic acid sodium water solution.
8, according to the forming method of the described high-strength ceramic composite materials gel injection moulding blank of claim 4, it is characterized in that: described initiator is an ammonium persulfate aqueous solution, or superoxol.
9, according to the forming method of the described high-strength ceramic composite materials gel injection moulding blank of claim 4, it is characterized in that: described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101618568B (en) * | 2009-02-27 | 2011-05-11 | 清华大学 | Preparation method of superfine ceramic powder injection molding mixture |
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| CN100449012C (en) * | 2007-03-08 | 2009-01-07 | 北京科技大学 | Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio |
| NO328397B1 (en) * | 2007-07-04 | 2010-02-08 | Yara Int Asa | Process for producing ceramic catalysts. |
| CN101892398B (en) * | 2010-07-01 | 2012-07-04 | 西安理工大学 | Method for preparing ceramic/aluminum alloy gradient composite material |
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Patent Citations (4)
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| CN1199102A (en) * | 1998-04-21 | 1998-11-18 | 冶金工业部钢铁研究总院 | Method for preparation of composite ceramic-Ni-Al intermetallic material |
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| CN101618568B (en) * | 2009-02-27 | 2011-05-11 | 清华大学 | Preparation method of superfine ceramic powder injection molding mixture |
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