CN100584795C - Mullite nano crystallite ceramic product and preparation method thereof - Google Patents
Mullite nano crystallite ceramic product and preparation method thereof Download PDFInfo
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- CN100584795C CN100584795C CN200710303412A CN200710303412A CN100584795C CN 100584795 C CN100584795 C CN 100584795C CN 200710303412 A CN200710303412 A CN 200710303412A CN 200710303412 A CN200710303412 A CN 200710303412A CN 100584795 C CN100584795 C CN 100584795C
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Abstract
The invention relates to a ceramic product of mullite nanometer microcrystalline and a preparation method thereof and comprises three materials: mullite, zirconium oxide and barium carbonate. The three materials are added with 10 percent of nucleating agent after proportioning, then being sent into a ball mill to be ground; next, the obtained material is dried to be a compound material that is then ground and melted in a high-melting furnace; the obtained material is clarified into a homogeneous glass melt; finally, the product is made through centrifugal casting or sintering technique. The crystal content of the mullite of the material is larger than or equal to 70 percent, and is less than or equal to 100nm; the draw strength is larger than or equal to 650 MPa, and the friction coefficient is less than or equal to 2 multiplied by 10<-3>. By using phase separation mechanism to form spherical mullite crystal, and adopting nucleating agent to initiate cylindrical mullite crystal, the uniformity of the invention is effectively ensured, thus guaranteeing properties of materials.
Description
Technical field
The present invention relates to a kind of mullite nano crystallite ceramic product and preparation method thereof.
Background technology
The widespread use on market of micro-crystalline ceramic material from the electromagnetic oven panel of tableware for daily use, kitchen range, is arrived highly sophisticated products such as gyrostat, precision optical instrument, guided missile head nose cone, and launch is all arranged.The tradition household china is to utilize in the base substrate part to form glassy phase to realize densification, and its densification degree is not high.
Developed mullite micro-crystalline ceramic material abroad, it is that to utilize mullite be AL
2O
3-SiO
2Unique stable compound in the binary system has the fusing point height, the high temperature resistance creep-resistant property is good, thermal expansivity is little, and stable chemical performance, is the good high temperature resistant structure ceramics of a kind of performance.But traditional preparation method exists complex process, compactness is poor, the shortcoming that mullite crystal content is low, the sintering shrinkability is big.
Summary of the invention
The objective of the invention is to overcome above-mentioned defective, provide that a kind of sintering shrinkability is little, crystal is evenly distributed, compactness good, mullite nano crystallite ceramic product that mullite crystal content is high and preparation method thereof.
Technical scheme of the present invention is: a kind of preparation method of mullite nano crystallite ceramic product is characterized in that described mullite nano crystallite ceramic product is by following powder material:
Mullite (3AL
2O
3.2SiO
2) 90～95 weight %
Zirconium white (ZrO
2) 3～5 weight %
Barium carbonate (BaCO
3) 2～5 weight %
Constitute;
Its preparation method comprises:
(1) with above-mentioned mullite, three kinds of powder materials of zirconium white and barium carbonate by proportioning and add after 10% nucleator slurry drops into ball mill grinding and become granularity≤100 orders, send into drying room and be dried to compound, drying temperature is≤200 ℃, drying time is 0.8～1.2 hour, making its water ratio is 2～3%, and its nucleator slurry is by yttrium oxide (Y
2O
3) and Silver Nitrate (AgNO
3) two kinds of mixed raw materials become;
(2) compound that (1) is obtained is sent into powder beater and is crushed to granularity≤80 orders;
(3) melt, clarify in the high-temperature melting furnace that the granularity that (2) are obtained≤80 purpose compounds are sent into, its melt temperature is 1800 ℃～2000 ℃, and the time length is 1.5～2.5 hours, the homogeneous glass melt that obtains;
(4) the homogeneous glass melt that (3) are obtained carries out rotational casting technology or sintering process acquisition mullite nano crystallite ceramic product, make the mullite crystal grain diameter≤100nm in its goods, rice stone crystalline content 〉=70% not, folding strength 〉=650MPa, frictional coefficient≤2 * 10
-3, its rotational casting technology is meant that large-scale rotational symmetry goods are to adopt the metal die rotational casting; And sintering process is meant that general goods or particular product are to adopt gel injection method molding blank, with graphite master form tool sintering;
A. rotational casting technology:
The homogeneous glass melt that (3) are obtained adopts the metal die rotational casting, the demoulding then, deburring obtain blank, again blank is sent into and carried out the crystallization processing in the stove, controlled temperature is 880 ℃～900 ℃, soaking time 12～20 hours, cooling then, temperature fall time is 10～12 hours, reduces to normal temperature and promptly obtains mullite nano crystallite ceramic product;
B. sintering process:
After the homogeneous glass melt that (3) are obtained carries out shrend, pulverize, its granularity≤100 orders adds 0.5～0.6 ‰ conventional sintering agent again and puddles evenly, adopt the slurrying of ordinary method gel, casting to obtain base substrate then, again base substrate is sent into and carried out the crystallization processing in the stove, adopt graphite master form tool sintering, controlled temperature 1600 ℃～1650, soaking time 1～3 hour, cooling then, temperature fall time is 5～6 hours, reduces to normal temperature and promptly obtains mullite nano crystallite ceramic product.
The present invention uses for reference the glassification process thinking, employing be the micro-crystalline ceramic production technique, after the material monolithic fusing, formed product is handled through crystallization, makes the abundant densification of material.The utilization parvafacies mechanism forms spherical mullite crystal, utilizes nucleator then can cause cylindrical mullite crystal.
Then the two combines with parvafacies mechanism and nucleator in the present invention, increasing the total quantity of mullite crystal, thereby has increased the strength of materials, reduces friction.In addition, nucleator adopts nanometer to handle, and fully disperses the back to add, and this technology guarantees homogeneity effectively, and because nucleator is tiny, helps forming the nano level mullite crystal.
The present invention is the growth of controlled oxidation aluminium and mullite crystal effectively, thereby makes the mullite crystal in the material be tiny needle-like, and is evenly distributed.
Big profile shaft to the glaze goods, is adopted rotational casting; For specialty products, adopt sintering process, then use gel injection method molding blank, with graphite master form tool sintering, the total contraction of this technology is little also very novel.
In sum, the principal crystalline phase of this micro-crystalline ceramic is a mullite crystal, and its folding strength is 1～2 times of common devitrified glass up to more than the 650MPa.And frictional coefficient is little, belongs to a kind of ideal friction resistant material, is widely used on Aeronautics and Astronautics and the rub resistance foundry goods, and every performance all is better than common devitrified glass.Material fully fine and close (void content closely zero), and integral body has good uniformity, and is better than other densification process technology, and for making massive article, these characteristics are particularly outstanding.Most of goods can adopt casting, blow, the pulling shaping explained hereafter, do not need post-treatment.Size is accurate, any surface finish.Under the special information condition, also available sinter molding.
Control batching and select correct nucleator by strictness, the fully clarification of fusing back, thermal treatment (nucleation and crystal growth) are controlled strict, crystal habit, quantity to material all can reach the expection requirement, and good reproducibility, thereby guarantee the performance of material, the good product quality of producing, the qualification rate height.
Embodiment:
Embodiment one (is example with large-scale rotational symmetry goods)
The preparation method of mullite nano crystallite ceramic product is by following powder material:
3AL
2O
3.SiO
295 weight %
ZrO
23 weight %
BaCO
32 weight %
Constitute;
Its preparation method comprises:
(1) with above-mentioned mullite (3AL
2O
3.2SiO
2), zirconium white (ZrO
2) and barium carbonate (BaCO
3) three kinds of powder materials are by proportioning and add after 10% nucleator slurry drops into ball mill grinding and become granularity≤100 orders, send into drying room and be dried to compound, drying temperature is≤200 ℃, drying time is 0.8～1.2 hour, make its water ratio less than 3%, its nucleator slurry is to be become with nitric acid money kind mixed raw material by yttrium oxide;
(2) compound that (1) is obtained is sent into powder beater and is crushed to granularity≤80 orders.
(3) granularity that (2) are obtained≤80 purpose compounds are sent in the high-temperature melting furnace and are melted, clarify, and its melt temperature is 1800 ℃～2000 ℃, and the time length is 2.5 hours, the homogeneous glass melt that obtains;
(4) the homogeneous glass melt that (3) are obtained carries out rotational casting technology acquisition mullite nano crystallite ceramic product, make the mullite crystal grain diameter≤100nm in its goods, mullite crystal content 〉=70%, folding strength 〉=650MPa, frictional coefficient≤2 * 10
-3,
Rotational casting technology:
The homogeneous glass melt that (3) are obtained adopts the metal die rotational casting, the demoulding then, deburring obtain blank, again blank is sent into and carried out the crystallization processing in the stove, controlled temperature is 880 ℃～900 ℃, soaking time 12～20 hours, cooling then, temperature fall time is 10～12 hours, reduces to normal temperature and promptly obtains mullite nano crystallite ceramic product;
Examples of implementation two (is example with specialty products)
The preparation method of mullite nano crystallite ceramic product is by following powder material:
3AL
2O
3.SiO
295 weight %
ZrO
23 weight %
BaCO
32 weight %
Constitute;
(1) with above-mentioned mullite (3AL
2O
3.2SiO
2), zirconium white (ZrO
2) and barium carbonate (BaCO
3) three kinds of powder materials are by proportioning and add after 10% nucleator slurry drops into ball mill grinding and become granularity≤100 orders, send into drying room and be dried to compound, drying temperature is≤200 ℃, drying time is 0.8～1.2 hour, make its water ratio less than 3%, its nucleator slurry is to be become with nitric acid money kind mixed raw material by yttrium oxide;
(2) compound that (1) is obtained is sent into powder beater and is crushed to granularity≤80 orders.
(3) granularity that (2) are obtained≤80 purpose compounds are sent in the high-temperature melting furnace and are melted, clarify, and its melt temperature is 1800 ℃～2000 ℃, and the time length is 2.5 hours, the homogeneous glass melt that obtains;
(4) the homogeneous glass melt that (3) are obtained carries out sintering process acquisition mullite nano crystallite ceramic product, makes the mullite crystal grain diameter≤100nm in its goods, mullite crystal content 〉=70%, folding strength 〉=650MPa, frictional coefficient≤2 * 10
-3,
Sintering process:
After the homogeneous glass melt that (3) are obtained carries out shrend, pulverize, its granularity≤100 orders adds 0.5～0.6 ‰ conventional sintering agent again and puddles evenly, adopt the slurrying of ordinary method gel, casting to obtain base substrate then, again base substrate is sent into and carried out the crystallization processing in the stove, adopt graphite master form tool sintering, controlled temperature 1600 ℃～1650, soaking time 1～3 hour, cooling then, temperature fall time is 5～6 hours, reduces to normal temperature and promptly obtains mullite nano crystallite ceramic product.
Claims (2)
1. the preparation method of a mullite nano crystallite ceramic product is characterized in that described mullite nano crystallite ceramic product is by following powder material:
3Al
2O
3SiO
290～95 weight %
ZrO
23～5 weight %
BaCO
32～5 weight %
Make;
Its preparation method comprises:
(1) with above-mentioned mullite, three kinds of powder materials of zirconium white and barium carbonate by proportioning and add after 10% nucleator slurry drops into ball mill grinding and become granularity≤100 orders, send into drying room and be dried to compound, drying temperature is≤200 ℃, drying time is 0.8～1.2 hour, making its water ratio is 2～3%, and its nucleator slurry is to be become with nitric acid money kind mixed raw material by yttrium oxide;
(2) compound that (1) is obtained is sent into powder beater and is crushed to granularity≤80 orders,
(3) granularity that (2) are obtained≤80 purpose compounds are sent in the high-temperature melting furnace and are melted, clarify, and its melt temperature is 1800 ℃～2000 ℃, and the time length is 1.5～2.5 hours, the homogeneous glass melt that obtains;
(4) the homogeneous glass melt that (3) are obtained carries out rotational casting technology or sintering process acquisition mullite nano crystallite ceramic product, make the mullite crystal grain diameter≤100nm in its goods, mullite crystal content 〉=70%, folding strength 〉=650MPa, frictional coefficient≤2 * 10
-3,
Described rotational casting technology is meant that large-scale rotational symmetry goods are to adopt the metal die rotational casting;
Described sintering process is meant that general goods or particular product are to adopt gel injection method molding blank, with graphite master form tool sintering;
A. rotational casting technology:
The homogeneous glass melt that (3) are obtained adopts the metal die rotational casting, the demoulding then, deburring obtain blank, again blank is sent into and carried out the crystallization processing in the stove, controlled temperature is 880 ℃～900 ℃, soaking time 12～20 hours, cooling then, temperature fall time is 10～12 hours, reduces to normal temperature and promptly obtains mullite nano crystallite ceramic product;
B. sintering process:
After the homogeneous glass melt that (3) are obtained carries out shrend, pulverize, its granularity≤100 orders adds 0.5～0.6 ‰ conventional sintering agent again and puddles evenly, adopt the slurrying of ordinary method gel, casting to obtain base substrate then, base substrate is sent into again and carried out the crystallization processing in the stove, adopt graphite master form tool sintering, controlled temperature is 1600 ℃～1650 ℃, soaking time is 1～3 hour, cooling then, temperature fall time is 5～6 hours, reduces to normal temperature and promptly obtains mullite nano crystallite ceramic product.
2. by the mullite nano crystallite ceramic product of the described method of claim 1 preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710303412A CN100584795C (en) | 2007-12-25 | 2007-12-25 | Mullite nano crystallite ceramic product and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710303412A CN100584795C (en) | 2007-12-25 | 2007-12-25 | Mullite nano crystallite ceramic product and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101186492A CN101186492A (en) | 2008-05-28 |
| CN100584795C true CN100584795C (en) | 2010-01-27 |
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| CN110862268B (en) * | 2019-12-04 | 2023-07-21 | 冷水江市汇鑫电子陶瓷有限公司 | Composite ceramic material and preparation method and application thereof |
| CN111484337B (en) * | 2020-04-15 | 2021-01-22 | 扬州爱斯派电器有限公司 | Sintering preparation process of microcrystalline ceramic plate |
| CN112794706A (en) * | 2021-02-05 | 2021-05-14 | 佛山陶者陶瓷技术有限公司 | High-strength ceramic plate and preparation method thereof |
| CN116606072B (en) * | 2023-07-20 | 2023-10-27 | 内蒙古兴固科技有限公司 | Preparation method of ultrathin ultra-wide nano microcrystalline plate |
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Granted publication date: 20100127 Termination date: 20131225 |