CN1242351A - Method for preparing high temp. refractory material special shaped parts by using quick solidification and shape-forming tech. - Google Patents
Method for preparing high temp. refractory material special shaped parts by using quick solidification and shape-forming tech. Download PDFInfo
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- CN1242351A CN1242351A CN 99109822 CN99109822A CN1242351A CN 1242351 A CN1242351 A CN 1242351A CN 99109822 CN99109822 CN 99109822 CN 99109822 A CN99109822 A CN 99109822A CN 1242351 A CN1242351 A CN 1242351A
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Abstract
The quick-solidifying and forming preparation method of high-temp. refractory material shaped component includes the following steps: firstly, mixing organic monomer and crosslinking agent with water, dissolving, then adding the powdered refractory material into the above-mentioned organic monomer aqueous solution, stirring and dispersing to prepare slurry material, then adding dispersing agent, stabilizing agent and defoaming agent, then adding initiating agent into the obtained suspension while stirring, and pouring the suspension into the mould, heating and heat-insulating so as to obtain the invented refractory material blank body. Said invented method has no contraction of volume in the solidifying and forming process of the slurry material, can obtain the refractory products with various shapes and different sizes, and their quality is good.
Description
The present invention relates to a kind of rapid solidification moulding preparation method of high-temperature refractory form parts, belong to the high-temperature refractory technical field.
High-temperature refractory is the high-temperature material of the class excellent performance that grows up on the basis of traditional ceramics and common refractory, and it has higher chemical purity, high fusing point (1700～4000 ℃), good chemical stability, thermostability and hot strength.Therefore, play a significant role at sciemtifec and technical spheres such as space flight, new forms of energy, reactor, special metallurgy.The for example liner of rocket combustion chamber and nozzle, magnetohydrodynamic generator channel material, the control rod of reactor intercept neutrons, metallurgical smelting pot, aircraft turbine blades etc.This type high temp refractory materials kind is many, complex-shaped, and dimensional precision and high-temperature behavior require high.Yet traditional molding method for preparing has been difficult to meet the demands at present.As existing compression molding, ramming method, the extrinsion pressing that uses, only be suitable for the better simply goods of shape; The gypsum mould grouting method also can only forming thin-walled goods, and is still very difficult for the moulding of the solid and complex-shaped high-temperature flame-proof parts of many thickness, usually causes molding blank top layer and center density and forms inconsistent and produce cracking.And the blank strength of gypsum mould grouting moulding is low, and dimensional precision and surface smoothness are also relatively poor.
The objective of the invention is to propose a kind of rapid solidification moulding preparation method of high-temperature refractory form parts, at first in the organic monomer aqueous solution, add solid powder and dispersion agent, prepare high solid loading (〉=suspensoid 50vol%) or slurry with flowability; Add initiator (or adding catalyzer simultaneously) then and mix.Again this mixed slurry is poured into a mould in the mould that does not into absorb water, postheating to 60～80 ℃, initiator causes the organic monomer polyreaction and forms three-dimensional network and makes that the slurry original position is frozen into the refractory materials base substrate in the die cavity.
The rapid solidification moulding preparation method of high-temperature refractory form parts of the present invention comprises following each step:
1, organic monomer (as acrylamide) and linking agent (as methylene-bisacrylamide) and water mixed dissolution, (monomer: linking agent=30～70: 1) preparing concentration is 2～50% the aqueous solution (claiming the monomer premixed liquid again).
2, the powder of refractory materials (SiC, Al
2O
3, zircon sand fine powder, Si
3N
4) add in the above-mentioned organic monomer aqueous solution and dispersed with stirring, prepare high solid volume fraction (〉=50vol%) slurry.Can add some dispersion agents for improving slurry fluidity.The dispersion agent that uses comprises polyacrylic acid, ammonium polyacrylate, Polyacrylamide, ammonium citrate, polyoxyethylene glycol.Dispersant dosage accounts for 0.5～2.0wt% of ceramic powder weight.Not sedimentation can add suspension stabilizer in order to guarantee slurry suspension to stablize, and as sodium alginate, methylcellulose gum, the add-on of suspension stabilizer accounts for 0.5～1wt% of solid powder.
3, after powder and dispersion agent and the aqueous solution mix, might produce a small amount of bubble; Can add some defoamers (as Virahol, lipid acid, tbp), stir a little and can eliminate bubble, the add-on of defoamer is 0.05～0.5wt%.
4, initiator (as POTASSIUM PERSULFATE or Ammonium Persulfate 98.5) is added in the above-mentioned suspensoid while stirring, the add-on of initiator is 0.05～1wt%, then this suspensoid cast is entered in the mould, moulding stock is non-hole materials such as metal, plastics, rubber, glass.For guaranteeing that suspensoid is full of mould, but the vibration while pouring into a mould.
5, heating mould to 60～80 ℃ then.About 10～60 minutes, suspensoid solidified fully, can obtain intact solidified refractory materials base substrate of the present invention.
Use the rapid solidification moulding preparation method of high-temperature refractory form parts of the present invention, have following advantage:
1) slurry coagulation forming process does not have volumetric shrinkage, is a kind of dead size moulding of in-situ solidifying;
2) fire resistive material product of plastic various complicated shape and different size size;
3) molding blank homogeneity height, quality are good;
4), make the intensity height, good toughness of base substrate after the moulding, cracky not because polymerization macromolecule and particulate keying action;
5) the product's dimensional precision height of moulding.
Introduce embodiments of the invention embodiment 1 below: the moulding of silicon nitride combined silicon carbide high-temperature flame-proof parts
Silicon nitride combined silicon carbide is the high-temperature refractory of excellent performance.It is synthetic through 1380 ℃ of-1450 ℃ of nitrogenizing reactions by the biscuit of metal Si powder and SiC granules preparation.Therefore, preparation high-density, inner Si/SiC base substrate uniformly are the application of this moulding process.The SiC raw material particle size is distributed as 50-500 μ m, and the Si powder directly is 10-100 μ m.
In 100 ml waters, add 10 gram acrylamides and 0.3 gram methylene-bisacrylamide, stir back dissolving rapidly.Add 350 gram Si powder and SiC particle (annotate, Si powder and SiC particle proportional range are respectively: Si powder 15-35%, SiC particle 65-85%) then.Add 0.2 ml polypropylene acid ammonium dispersion agent again.Coarse particles sinks among the SiC in order to avoid, and adds the sodium alginate polymer of 0.1 gram, obtains homodisperse concentrated suspension, adds micro-tbp and eliminates bubble.Add 0.2 milliliter of ammonium persulfate initiator then in slurry.Slurry is heated to 70 ℃ after injecting mould.After 15 minutes, promptly be solidified into difform biscuit.
Embodiment 2: zircon high-temperature flame-proof parts-moulding
With the natural zircon sand fine powder after the calcining is raw material.In 100 milliliters premixed liquids (80wt% water+20wt% acrylamide monomer+0.5wt% methylene-bisacrylamide), add 500 gram zircons.For improving dispersiveness, add the 1wt% polyacrylic acid dispersant, fully stir, the initiator potassium persulfate with 300 microlitres joins in the slurry restir then.The defoamer that adds a small amount of Virahol class lower alcohol is simultaneously removed issuable bubble in the stirring.Above-mentioned slurry is injected a metal die, put into 60 ℃ of baking ovens.About 40 minutes slurry curings become the base substrate of desired shape.
Embodiment 3: the preparation of corundum refractory parts-moulding
Corundum refractory is with Al
2O
3For main component (contains Al
2O
3More than 90%), corundum is the refractory product of crystalline phase, is widely used on the chemical metallurgy, used raw material is a lapis amiridis.
The lapis amiridis granularity is 30-200 μ m.In 250 milliliters of monomer premixed liquids (85wt% water+15wt% acrylamide monomer+0.25wt% methylene-bisacrylamide), add 1000 gram lapis amiridiss, add 10 gram ammonium citrate dispersion agents simultaneously.For avoiding the sedimentation of a small amount of corundum coarse particles, add the methylcellulose gum polymer and the abundant dispersed with stirring of about 0.2 gram, make solid volume fraction and be about 50% slurry.Froth in vacuum adds 700 microlitre initiator Ammonium Persulfate 98.5s subsequently in slurry then.Stir and to inject mould after being uniformly dispersed in 5 minutes.Heating mould to 70 ℃.About 20 minutes, slurry curing was shaped to the parts of desired shape.
Embodiment 4: reaction sintering Si
3N
4The preparation of high-temperature refractory parts biscuit
Reaction sintering Si
3N
4The raw material of goods adopts metallic silicon power, and silica flour (Si) is at 1360-1450 ℃ and N
2Reaction generates high temperature Si
3N
4Crystalline phase.Key is the difform silica flour biscuit of preparation.
The silica flour raw material is two kinds of particle diameters of 2 μ m and 20 μ m.In 250 gram premixed liquids (65wt% water+34wt% acrylamide monomer+1wt% methylene-bisacrylamide), add 700 gram silica flours, add weakly alkaline or neutral dispersion agent simultaneously, as ammonium polyacrylate.Mechanical stirring was disperseed after 20 minutes, by vibrating and adding a small amount of bubble that fatty acid defoamer is removed slurry, added initiator potassium persulfate 650 microlitres then, and stirred.At room temperature (20-25 ℃) injects mould with slurry, and the baking oven of putting into 60-80 ℃ heated 30 minutes, and slurry is the curable base substrate that obtains definite shape.
Claims (4)
1, a kind of rapid solidification moulding preparation method of high-temperature refractory form parts is characterized in that, this method comprises following each step:
(1) with organic monomer acrylamide and linking agent methylene-bisacrylamide and water mixed dissolution, monomer: linking agent=30～70: 1, preparing concentration and be 2～50% the aqueous solution is the monomer premixed liquid;
(2) powder with refractory materials adds in the above-mentioned organic monomer aqueous solution and dispersed with stirring, prepare the slurry of high solid volume fraction 〉=50vol%, and adding dispersion agent, dispersant dosage accounts for 0.5～2.0wt% of ceramic powder weight, adding suspension stabilizer sodium alginate or methylcellulose gum, account for 0.05～1wt% of solid powder with the consumption of suspension stabilizer;
(3) after powder and dispersion agent and the aqueous solution mix, add defoamer again, defoamer accounts for 0.05～0.5wt% of solid powder;
(4) initiator POTASSIUM PERSULFATE or Ammonium Persulfate 98.5 are added in the above-mentioned suspensoid while stirring, the add-on of initiator accounts for 0.05～1wt% of solid powder, then this suspensoid cast is entered in the mould vibration while pouring into a mould;
(5) at last with mold heated to 60～80 ℃, be incubated 10～60 minutes, suspensoid solidifies fully, is curing refractory materials base substrate of the present invention.
2, the method for claim 1 is characterized in that, wherein said refractory materials is SiC, Al
2O
3, zircon sand fine powder, Si
3N
4In any.
3, the method for claim 1 is characterized in that, wherein said dispersion agent is any in polyacrylic acid, ammonium polyacrylate, the ammonium citrate.
4, the method for claim 1 is characterized in that, wherein said defoamer is any in Virahol, lipid acid, the tbp.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99109822 CN1242351A (en) | 1999-07-16 | 1999-07-16 | Method for preparing high temp. refractory material special shaped parts by using quick solidification and shape-forming tech. |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99109822 CN1242351A (en) | 1999-07-16 | 1999-07-16 | Method for preparing high temp. refractory material special shaped parts by using quick solidification and shape-forming tech. |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1131186C (en) * | 2000-12-29 | 2003-12-17 | 清华大学 | Colloid injection method and equipment for shaping ceramics |
| CN1293022C (en) * | 2005-03-02 | 2007-01-03 | 中国航空工业第一集团公司北京航空材料研究院 | Preparation method of honeycomb ceramic mud blank |
| CN101880166A (en) * | 2010-06-13 | 2010-11-10 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN101928143A (en) * | 2010-08-24 | 2010-12-29 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-purity zirconia refractory product |
| CN101514107B (en) * | 2009-03-13 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Mixed initiating system for increasing the stability of gelatin casting molding ceramic slurry and use method thereof |
| CN104446291A (en) * | 2014-10-21 | 2015-03-25 | 北京科技大学 | Preparation method for preparing panel by using desulfurization gypsum |
| CN113429209A (en) * | 2021-06-16 | 2021-09-24 | 咸阳陶瓷研究设计院有限公司 | Preparation method of high solid-phase content barren grouting material for desulfurization nozzle |
| CN114524678A (en) * | 2022-02-25 | 2022-05-24 | 江苏东台超凡创新新材料科技有限公司 | Alumina-silicon carbide-carbon refractory material prepared from aluminum ash and preparation method thereof |
-
1999
- 1999-07-16 CN CN 99109822 patent/CN1242351A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1131186C (en) * | 2000-12-29 | 2003-12-17 | 清华大学 | Colloid injection method and equipment for shaping ceramics |
| CN1293022C (en) * | 2005-03-02 | 2007-01-03 | 中国航空工业第一集团公司北京航空材料研究院 | Preparation method of honeycomb ceramic mud blank |
| CN101514107B (en) * | 2009-03-13 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Mixed initiating system for increasing the stability of gelatin casting molding ceramic slurry and use method thereof |
| CN101880166A (en) * | 2010-06-13 | 2010-11-10 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN101880166B (en) * | 2010-06-13 | 2013-05-08 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN101928143A (en) * | 2010-08-24 | 2010-12-29 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-purity zirconia refractory product |
| CN101928143B (en) * | 2010-08-24 | 2012-12-26 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-purity zirconia refractory product |
| CN104446291A (en) * | 2014-10-21 | 2015-03-25 | 北京科技大学 | Preparation method for preparing panel by using desulfurization gypsum |
| CN113429209A (en) * | 2021-06-16 | 2021-09-24 | 咸阳陶瓷研究设计院有限公司 | Preparation method of high solid-phase content barren grouting material for desulfurization nozzle |
| CN114524678A (en) * | 2022-02-25 | 2022-05-24 | 江苏东台超凡创新新材料科技有限公司 | Alumina-silicon carbide-carbon refractory material prepared from aluminum ash and preparation method thereof |
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