CN101182208A - Nano multi-phase high-temperature material - Google Patents
Nano multi-phase high-temperature material Download PDFInfo
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- CN101182208A CN101182208A CNA2007101683509A CN200710168350A CN101182208A CN 101182208 A CN101182208 A CN 101182208A CN A2007101683509 A CNA2007101683509 A CN A2007101683509A CN 200710168350 A CN200710168350 A CN 200710168350A CN 101182208 A CN101182208 A CN 101182208A
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Abstract
The invention relates to a nanometer functional material and the electric heating technical field and concretely relates to a nanometer complex phase high-temperature ceramic material and film material. The components and the weight percentage contents of the components of the invention are 60 percent to 80 percent of main crystal phase and 20 percent to 40 percent of the mixture powder of nanometer grade yttrium hydroxide and aluminum hydroxide, or the components of the invention comprises the main crystal phase, the mixture powder of nanometer grade yttrium hydroxide and aluminum hydroxide, a binder phase and organic solvent. The binder phase is submicron grade lead-free glass powder which is made by milling the lead-free glass powder by a high-energy ball mill device; the main crystal phase is submicron grade powder silicon made by the high-energy ball mill device. The nanometer complex phase high-temperature material of the invention has the effects as follows: the heating temperature is high; the raw material does not contain the toxicants such as lead, hydrargyrum, cadmium, hexavalent chromium, polybrominated diphenyl ether, benzene etc., the material causes no environmental pollution and belongs to the environmental protective material; the infrared radiant energy and the electricity-heat radiation conversion efficiency are high; the performance of heat-impact resistance is good.
Description
Technical field
The present invention relates to nano-functional material and electric-heating technology field, concrete relate to a kind of nano multi-phase high-temperature material.
Background technology
The sight field that claims to be situated between, the field between microcosmic and the macroscopical field of being in studies show that many surprised, peculiar physics, chemical property that this field occurs make human recognition for objective world to be advanced to a new stage.Jie's sight field comprises that cluster, nanometer and submicron system form zero dimension, one dimension, two dimension, three-dimensional material.Wherein the nanoparticle of most of nano materials only contains a limited number of brilliant bag, do not have periodically, and the energy of surface atom is several times of inner nuclear energy.
Because nano grain surface can be high, surface particle is many, and is active high, required little energy during the nano particle fusing, and fusing point descends, and sintering temperature reduces.Like this, the energy-saving effect highly significant in the production link.
Preparation of nanomaterials has chemical precipitation method, sol-gel method, hydrothermal method, high-energy ball milling method, ammonia nitriding or the like.The preparation of stupalith must be passed through high temperature sintering, the recrystallization of crystal grain at this moment will inevitably occur.This brings difficulty can for the preparation of single phase nano material.If in the body material of external phase, add nano level second, third phase material, as disperse the mutual-assistance it when being present in the intragranular of body material or the crystal boundary, form the nanometer composite diphase material, situation will change to some extent.It not only can make material toughness reinforcing, strengthens, and can also make material have multi-functional effect, so nano heterogeneous ceramic just becomes the nano ceramics that has practical value most.
Yttrium aluminum garnet (Y
3Al
5O
12) have garnet structure, be the best oxidation-resistant material of creep resistance known at present.Yttrium aluminum garnet and aluminum oxide (Al
2O
3) they have good chemical compatibility, similar thermal expansivity and high-melting-point very, and very strong oxidation-resistance is arranged.Therefore the matrix material of yttrium aluminum garnet and aluminum oxide is a kind of material of high-temperature-resistant structure well.
The existing heating unit for preparing with the conditional electronic ceramic process with powder silicon (Si) and additive, the electric heating property with every excellence.But heating temp high not enough (700-800) ℃, antioxidant property is strong not enough, and especially high-temperature stability is relatively poor.
Summary of the invention
The objective of the invention is to propose a kind of nano multi-phase high-temperature material at above-mentioned prior art, its objective is the deficiency that overcomes existing thermo electric material, bringing into play better with silicon is the characteristic of the heating material of matrix.
Another object of the present invention is the preparation method who proposes nano multi-phase high-temperature material.
Nanometer complex phase high temperature ceramic material, the quality percentage composition of its component and component is a principal crystalline phase 60~80%, nano level yttrium hydroxide and alumag powder 20~40%, described principal crystalline phase are the submicron order powder silicon that adopts high-energy ball milling equipment to make.
Described nano level yttrium hydroxide and alumag powder are prepared from by following method: the mixed that at first with aluminum nitrate, Yttrium trinitrate is 3: 5 in molar ratio, and adding distilled water fully dissolves it, be mixed with Yttrium trinitrate, the mixed solution of aluminum nitrate adds ammoniacal liquor again, makes its precipitation, after reacting completely, through dehydration, obtain nano level yttrium hydroxide and alumag, obtain nano level yttrium hydroxide and alumag powder after the oven dry.
The preparation method of nanometer complex phase high temperature ceramic material, with nano level yttrium hydroxide and alumag powder after being mixed in proportion with principal crystalline phase, obtain nanometer complex phase high temperature ceramic material through granulation, moulding, high temperature sintering, described sintering temperature is 1000-1300 ℃, nano level yttrium hydroxide and alumag powder have formed nano level yttrium aluminum garnet and aluminum oxide during sintering, and are in the crystal boundary of principal crystalline phase and become the crystal boundary phase.
Nanometer complex phase high temperature membrane material, its component includes principal crystalline phase, nano level yttrium hydroxide and alumag powder, bonding phase and organic solvent, principal crystalline phase, the nano level yttrium hydroxide is collectively referred to as the solid phase mutually with alumag powder and bonding, principal crystalline phase wherein, nano level yttrium hydroxide and alumag powder and bonding solid mutually in shared mass percent be principal crystalline phase 50-60%, nano level yttrium hydroxide and alumag powder 5-35%, bonding phase 5-45%, the quality of solid phase and the volume ratio of organic solvent are: 100g: (82~400) ml, described bonding is submicron order crown glass powder mutually, being milled through high-energy ball milling equipment by the crown glass powder forms, and described principal crystalline phase is the submicron order powder silicon that adopts high-energy ball milling equipment to make.
Described nano level yttrium hydroxide and alumag powder are prepared from by following method: the mixed that at first with aluminum nitrate, Yttrium trinitrate is 3: 5 in molar ratio, and adding distilled water fully dissolves it, be mixed with Yttrium trinitrate, the mixed solution of aluminum nitrate adds ammoniacal liquor again, makes its precipitation, after reacting completely, through dehydration, obtain nano level yttrium hydroxide and alumag, obtain nano level yttrium hydroxide and alumag powder after the oven dry.
Described crown glass powder is to be produced by New Orient, Beijing science and technology Group Plc, and product type is DM-305, and physicals is as follows:
Product type | DM-305 |
The coefficient of expansion (1/ ℃) | 50.0×10 -7 |
Density (g/cm 3) | 2.2533 |
Softening temperature (℃) | 710 |
Press such scheme, described organic solvent is: Sodium hexametaphosphate 99, tbp, butyl carbitol amyl acetate, turps, rosinol, pimelinketone, Virahol, Terpineol 350, propyl carbinol, dibutyl phthalate (DBP), glycerol, Yelkin TTS, Viscotrol C, the multiple mixing of ethyl cellulose;
Described nanometer complex phase high temperature membrane preparation methods is that principal crystalline phase, nano level yttrium hydroxide are mixed in proportion mutually with alumag powder, bonding, mill, add organic solvent again and form the film slurry, through printing, spray or flooding with the matrix surface of slurry coating at silica glass, alumina ceramics or chemical porcelain, form the nontoxic nanometer complex phase high temperature membrane material that has from limitting temperature function again behind high temperature sintering, described sintering temperature is 900-1300 ℃.
Nano multi-phase high-temperature material of the present invention has following effect:
(1) heating temp is from room temperature to 1000 degree centigrade;
(2) resistivity of stupalith is that 0.1 Ω cm~10.0K Ω cm changes, and side's resistance of mould material is 0.1 Ω/~100.0K Ω/;
(3) temperature factor α T is 700~3000ppm/ ℃;
(4) toxic substances such as not leaded, the mercury of starting material, cadmium, sexavalent chrome, poly-dibromodiphenyl ether, benzene, non-environmental-pollution belongs to ep-type material;
(5) this material has high infrared energy and high electricity-thermal radiation efficiency of conversion;
(6) thermal shock resistance is good, and the heating temp maximum of nanometer multiple phase ceramic heating material can reach 1000 ℃ among the present invention; The heating temp maximum of nanometer complex phase electrothermal film material can reach 900-1000 ℃; High-temperature stability is good.
(7) this material can be depressed use in safety voltages such as 5V, 12V, 24V, 36V or 110V, 220V, 380V alternating current-direct current.
Embodiment
Embodiment one
Preparation nanometer complex phase high temperature ceramic material is pressed principal crystalline phase: nano level yttrium hydroxide and alumag powder=enforcement in 60%: 40%.
Principal crystalline phase is the submicron order silica flour body of milling and obtaining through high energy ball mill.
The preparation of nano level yttrium hydroxide and alumag powder: with 3: 5 in molar ratio mixed of precursor aluminum nitrate, Yttrium trinitrate, and adding distilled water fully dissolves it, be mixed with Yttrium trinitrate, the mixed solution of aluminum nitrate adds ammoniacal liquor again, make its precipitation, after reacting completely, through dehydration, become nano level aluminium hydroxide and yttrium hydroxide mixture again, drying forms aluminium hydroxide and yttrium hydroxide mixed powder, can deposit stand-by.
With the principal crystalline phase of jack mix with the alumag powder with the nano level yttrium hydroxides of 40 grams, granulation, moulding, at 1000-1200 ℃ of sintering temperature, formation has the nanometer complex phase high temperature ceramic material of electrical property.Coat the silver slurry at two end faces of material, become silver electrode 800 ℃ of following burning infiltrations again, just can form nano heterogeneous ceramic thermo electric material with electric heating function.
Detect the electrical property of its nano heterogeneous ceramic thermo electric material: resistivity is (500-10K) Ω cm, and heating temp 800-900 ℃, temperature factor α T is 700~1000ppm/ ℃.
Embodiment two
Preparation nano heterogeneous ceramic thermo electric material is pressed principal crystalline phase: nano level yttrium hydroxide and alumag powder=enforcement in 80%: 20%.
With the principal crystalline phase of quality 80 gram mix with the alumag powder with the nano level yttrium hydroxides of 20 grams, granulation, moulding, at 1000-1200 ℃ of sintering temperature, formation has the nanometer complex phase high temperature ceramic material of electrical property.Coat silver slurry at two end faces of material, become silver electrode 800 ℃ of following burning infiltrations again, just can form nano heterogeneous ceramic thermo electric material with electric heating function.
Detect the electrical property of its nano heterogeneous ceramic thermo electric material: resistivity is (50-500) Ω cm, and heating temp 800-900 ℃, temperature factor α T is 1000~2000ppm/ ℃.
Embodiment three
Preparation nano heterogeneous ceramic thermo electric material is pressed principal crystalline phase: nano level yttrium hydroxide and alumag powder=enforcement in 70%: 30%.
With the principal crystalline phase of quality 70 gram mix with the alumag powder with the nano level yttrium hydroxides of 30 grams, granulation, moulding, at 1000-1300 ℃ of sintering temperature, formation has the nanometer complex phase high temperature ceramic material of electrical property.Coat silver slurry at two end faces of material, become silver electrode 800 ℃ of following burning infiltrations again, just can form nano heterogeneous ceramic thermo electric material with electric heating function.
Detect the electrical property of its nano heterogeneous ceramic thermo electric material: resistivity is (0.1-500) Ω cm, and heating temp 800-1000 ℃, temperature factor α T is 1000-3000ppm/ ℃.
Embodiment four
Preparation nanometer complex phase high temperature membrane material, principal crystalline phase, nano level yttrium hydroxide are pressed enforcement in 60%: 35%: 5% with alumag powder, bonding mass ratio mutually.Wherein bonding is the submicron order powder that lead-free glass powder is milled and formed through high-energy ball milling equipment mutually.
Composition 10 examples (volume percent) of organic solvent:
Numbering | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
Rosinol | 73 | 8 | ||||||||
Turps | 3 | 60 | ||||||||
Terpineol 350 | 65 | 15 | 64 | 60 | 40 | 9 | 26 | |||
Pimelinketone | 14 | 17 | 71 | 65 | 14 | 10 |
Sodium hexametaphosphate 99 | 0.5 | 1.0 | 1.5 | |||||||
Tbp | 0.5 | 0.5 | 1.5 | 1.0 | 0.5 | |||||
Propyl carbinol | 14 | 17.5 | 10 | 10 | 10 | |||||
Ethyl cellulose | 4 | 3 | 4 | 4 | 3 | 4 | 3 | 3 | 3 | |
Yelkin TTS | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | |||||
The butyl carbitol amyl acetate | 3 | 4 | 2 | 5 | 3 | |||||
Dibutyl phthalate (DBP) | 2 | 3 | 3.5 | 19 | 19 | 2 | ||||
Ethanol | 10 | 7 | 40 | 60 | 54 | |||||
Viscotrol C | 1 | 9 | 15 | 5 | ||||||
Glycerol | 2 | 2 | 2 | 3 | 2 | 3 | 1.5 | 2 |
The principal crystalline phase of jack is mixed mutually with the yttrium aluminium hydroxide mixture powder of 35 grams and the bonding of 5 grams, total mass is 100 grams, adding the organic solvent of organic solvent the 6th example, is 400 milliliters by the quality of solid phase and the volume ratio of organic solvent for the organic solvent total amount.
Organic solvent (volume percent)
Total amount (ml) | Terpineol 350 (ml) | Tbp (ml) | Propyl carbinol (ml) | Ethyl cellulose (g) | Dibutyl phthalate (DBP) (ml) | Glycerol (ml) |
100 | 64 | 1.0 | 10 | 3 | 19 | 3 |
400 | 256 | 4.0 | 40 | 12 | 76 | 12 |
With solid with after organic solvent mixes, form nanometer complex phase high temperature membrane slurry through fully stirring the companion, through the spraying or the impregnating method with the matrix surface of slurry coating at silica glass, alumina ceramics or chemical porcelain, form the nontoxic nanometer complex phase high temperature membrane material that has from limitting temperature function behind high temperature sintering, wherein sintering temperature is 900-1200 ℃.Coat the silver slurry at the two ends of gained material, become silver electrode 800 ℃ of following burning infiltrations again, just can form nanometer complex phase electrothermal film material with electric heating function.
Detect the electrical property of its nano heterogeneous ceramic electrothermal film material: side's resistance is (1-500) Ω/, and heating temp 800-900 ℃, temperature factor α T is 1000~2000ppm/ ℃.
Embodiment five
Principal crystalline phase, nano level yttrium hydroxide are pressed enforcement in 50%: 5%: 45% with alumag powder, bonding mass ratio mutually.
Principal crystalline phase 50 grams, nano level yttrium hydroxide 45 restrain mutually with alumag powder 5 grams, bonding, solid phase total mass is 100 grams, adding the organic solvent of organic solvent the 2nd example, is 82 milliliters by the quality of solid phase and the volumetric ratio of organic solvent for the organic solvent total amount.
Organic solvent the 2nd example
Cubic capacity (ml) | Rosinol (ml) | Pimelinketone (ml) | Butyl carbitol amyl acetate (ml) | Dibutyl phthalate (DBP) (ml) | Viscotrol C (ml) | Glycerol (ml) |
100 | 73 | 17 | 4 | 3 | 1 | 2 |
82 | 60 | 14 | 3 | 2 | 1 | 2 |
With solid with after organic solvent mixes, form nanometer complex phase high temperature membrane slurry through fully stirring the companion, through printing process with the matrix surface of slurry coating at silica glass, alumina ceramics or chemical porcelain, form the nontoxic high temperature membrane material that has from limitting temperature function behind high temperature sintering, wherein sintering temperature is 900-1200 ℃.Coat the silver slurry at the two ends of material, become silver electrode 800 ℃ of following burning infiltrations again, just can form nanometer complex phase electrothermal film material with electric heating function.
Detect the electrical property of its nano heterogeneous ceramic electrothermal film material: side's resistance is (10-5000) Ω/, and heating temp 800-900 ℃, temperature factor α T is 700~2000ppm/ ℃.
Embodiment six
Principal crystalline phase, nano level yttrium hydroxide are pressed enforcement in 55%: 30%: 15% with alumag powder, bonding mass ratio mutually.
Principal crystalline phase 55 grams, nano level yttrium hydroxide 15 restrain mutually with alumag powder 30 grams, bonding, solid phase total mass is 100 grams, adding the organic solvent of organic solvent the 10th example, is 300 milliliters by the quality of solid phase and the volume ratio of organic solvent for the organic solvent total amount.
Organic solvent the 10th example
Cumulative volume (ml) | Terpineol 350 (ml) | Pimelinketone (ml) | Ethyl cellulose (ml) | Dibutyl phthalate (DBP) (ml) | Viscotrol C (ml) | Ethanol (ml) |
100 | 26 | 10 | 3 | 2 | 5 | 54 |
300 | 78 | 30 | 9 | 6 | 15 | 162 |
With solid with after organic solvent mixes, form nanometer complex phase high temperature membrane slurry through fully stirring the companion, through spraying, dipping method is the matrix surface of slurry coating at silica glass, alumina ceramics or chemical porcelain, form the nontoxic high temperature membrane material that has from limitting temperature function behind high temperature sintering, wherein sintering temperature is 900-1300 ℃.Coat the silver slurry at the two ends of material, become silver electrode 800 ℃ of following burning infiltrations again, just can form nanometer complex phase electrothermal film material with electric heating function.
Detect the electrical property of its nano heterogeneous ceramic electrothermal film material: side's resistance is (0.1-50) Ω/, and heating temp 800-1000 ℃, temperature factor α T is 1500~3000ppm/ ℃.
Claims (8)
1. nano multi-phase high-temperature material, the quality percentage composition that it is characterized in that its component and component is a principal crystalline phase 60~80%, nano level yttrium hydroxide and alumag powder 20~40%, described principal crystalline phase are the submicron order powder silicon that adopts high-energy ball milling equipment to make.
2. nano multi-phase high-temperature material according to claim 1, it is characterized in that described nano level yttrium hydroxide and alumag powder are prepared from by following method: the mixed that at first is 3: 5 in molar ratio with aluminum nitrate, Yttrium trinitrate, and adding distilled water fully dissolves it, be mixed with Yttrium trinitrate, the mixed solution of aluminum nitrate, add ammoniacal liquor again, make its precipitation, after reacting completely, through dehydration, obtain nano level yttrium hydroxide and alumag, obtain nano level yttrium hydroxide and alumag powder after the oven dry.
3. the preparation method of the described nano multi-phase high-temperature material of claim 1, it is characterized in that nano level yttrium hydroxide and alumag powder after being mixed in proportion with principal crystalline phase, through granulation, moulding, high temperature sintering, described sintering temperature is 1000-1300 ℃, nano level yttrium hydroxide and alumag powder have formed nano level yttrium aluminum garnet and aluminum oxide during sintering, and are in the crystal boundary of principal crystalline phase and become the crystal boundary phase.
4. nano multi-phase high-temperature material, it is characterized in that its component includes principal crystalline phase, nano level yttrium hydroxide and alumag powder, bonding phase and organic solvent, principal crystalline phase, the nano level yttrium hydroxide is collectively referred to as the solid phase mutually with alumag powder and bonding, principal crystalline phase wherein, nano level yttrium hydroxide and alumag powder and bonding solid mutually in shared mass percent be principal crystalline phase 50-60%, nano level yttrium hydroxide and alumag powder 5-35%, bonding phase 5-45%, the quality of solid phase and the volume ratio of organic solvent are 100g: 82~400ml, described bonding is submicron order crown glass powder mutually, being milled through high-energy ball milling equipment by the crown glass powder forms, and described principal crystalline phase is the submicron order powder silicon that adopts high-energy ball milling equipment to make.
5. nano multi-phase high-temperature material according to claim 4, it is characterized in that described nano level yttrium hydroxide and alumag powder are prepared from by following method: the mixed that at first is 3: 5 in molar ratio with aluminum nitrate, Yttrium trinitrate, and adding distilled water fully dissolves it, be mixed with Yttrium trinitrate, the mixed solution of aluminum nitrate, add ammoniacal liquor again, make its precipitation, after reacting completely, through dehydration, obtain nano level yttrium hydroxide and alumag, obtain nano level yttrium hydroxide and alumag powder after the oven dry.
6. according to claim 4 or 5 described nano multi-phase high-temperature materials, it is characterized in that described crown glass powder is to be produced by New Orient, Beijing science and technology Group Plc, product type is DM-305.
7. according to claim 4 or 5 described nano multi-phase high-temperature materials, it is characterized in that described organic solvent is: multiple mixing in Sodium hexametaphosphate 99, tbp, butyl carbitol amyl acetate, turps, rosinol, pimelinketone, Virahol, Terpineol 350, propyl carbinol, dibutyl phthalate (DBP), glycerol, Yelkin TTS, Viscotrol C or the ethyl cellulose.
8. the preparation method of the described nano multi-phase high-temperature material of claim 4, it is characterized in that principal crystalline phase, nano level yttrium hydroxide are mixed in proportion mutually with alumag powder, bonding, mill, add organic solvent again and form the film slurry, through printing, spray or flooding with the matrix surface of slurry coating at silica glass, alumina ceramics or chemical porcelain, form the nontoxic nanometer complex phase high temperature membrane material that has from limitting temperature function again behind high temperature sintering, described sintering temperature is 900-1300 ℃.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101902846A (en) * | 2010-07-21 | 2010-12-01 | 张福民 | Nano-silicon conductive ceramic electrical heating tube element and manufacture method thereof |
CN104764781A (en) * | 2015-03-31 | 2015-07-08 | 北京博曼迪汽车科技有限公司 | Electrode slurry and oxygen sensor |
CN112573826A (en) * | 2020-12-14 | 2021-03-30 | 佛山市东鹏陶瓷有限公司 | Energy powder, preparation method of deodorizing brick, deodorizing glaze and preparation method of deodorizing glaze |
-
2007
- 2007-11-15 CN CN200710168350A patent/CN100577604C/en not_active Expired - Fee Related
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101902846A (en) * | 2010-07-21 | 2010-12-01 | 张福民 | Nano-silicon conductive ceramic electrical heating tube element and manufacture method thereof |
CN104764781A (en) * | 2015-03-31 | 2015-07-08 | 北京博曼迪汽车科技有限公司 | Electrode slurry and oxygen sensor |
CN104764781B (en) * | 2015-03-31 | 2017-07-11 | 北京博曼迪汽车科技有限公司 | A kind of electrode slurry and lambda sensor |
CN112573826A (en) * | 2020-12-14 | 2021-03-30 | 佛山市东鹏陶瓷有限公司 | Energy powder, preparation method of deodorizing brick, deodorizing glaze and preparation method of deodorizing glaze |
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