CN103160148A - Surface-modified metal boride/Al2O3 multiphase ceramic powder and preparation method thereof - Google Patents
Surface-modified metal boride/Al2O3 multiphase ceramic powder and preparation method thereof Download PDFInfo
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- CN103160148A CN103160148A CN2013100787309A CN201310078730A CN103160148A CN 103160148 A CN103160148 A CN 103160148A CN 2013100787309 A CN2013100787309 A CN 2013100787309A CN 201310078730 A CN201310078730 A CN 201310078730A CN 103160148 A CN103160148 A CN 103160148A
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Abstract
The invention provides surface-modified metal boride/Al2O3 multiphase ceramic powder and a preparation method thereof. The surface-modified metal boride/Al2O3 multiphase ceramic powder has high performances and good interface compatibility with an organic resin and is subjected to organic functional group chemical-bonding surface modification. The preparation method comprises that metal boride/Al2O3 multiphase ceramic powder is subjected to organic functional group chemical-bonding surface modification to form the surface-modified metal boride/Al2O3 multiphase ceramic powder of which the surface is connected with organic functional groups by chemical bonding. The preparation method utilizes a coupling agent as a surface modifier. Inorganic philic groups in the coupling agent and surfaces of the metal boride/Al2O3 multiphase ceramic powder undergo a hydroxylation reaction so that through the hydroxylation reaction, the inorganic philic groups in the coupling agent are connected to the surfaces of the metal boride/Al2O3 multiphase ceramic powder and thus organic functional surface modification of the metal boride/Al2O3 multiphase ceramic powder is realized. The metal boride/Al2O3 multiphase ceramic powder subjected to organic functional group chemical-bonding surface modification and having high performances has good interfacial compatibility with an organic resin, high heat resistance and high wear resistance. The preparation method has simple processes, is convenient for operation and is conducive to industrial practical application.
Description
Technical field
The invention belongs to multiphase ceramic powder process for modifying surface field, relate to a kind of metal boride/aluminium sesquioxide (Al of surface modification
2O
3) multiphase ceramic powder and preparation method thereof, being specially provides a kind of and has good interface compatibility and greatly improve the surface of organic resin thermotolerance, wear resistance through the metal boride/Al of organic functional group chemical bonding modification with organic resin
2O
3Multiphase ceramic powder and preparation method thereof.
Background technology
The inorganic ceramic powder is filled with the performances such as thermal characteristics, mechanical property and tribology that the performance such as the high flexibility, workability of mechanical property, wear and corrosion behavior and high heat conduction resistance toheat and organic resin that the machine resin merged the inorganic ceramic excellence can significantly improve organic resin material, has caused domestic and international investigator's extensive attention since coming out always.The interface compatibility of inorganic ceramic powder and organic resin is the important factor of restriction potting resin component property performance.Research finds, and is poor when interface compatibility, and the inorganic ceramic powder can not be good when being dispersed in organic resin, and mineral filler just can not effectively be brought into play the effect that it improves the organic resin performance.Therefore, give full play to the function of high-performance inorganic ceramic packing, the performance of the organic resin of its filling is strengthened greatly, improving interface compatibility is the important topic of this area research.Because the inorganic ceramic powder is incompatible with the organic resin structure, common interface compatibility both is very poor, by the modification of inorganic ceramic powder surface organic functional group, improve the structural similarity of inorganic powder and organic resin, and then improve its interface compatibility at present by the confirmation of certain institute.But from previous research, the organically-modified research of inorganic ceramic powder surface focuses mostly in one-component ceramic, as SiO
2, Al
2O
3, SiC and TiO
2Deng, for complex phase ceramic research also the research of carrying out the organic functional group modification of rarely found report, particularly metal boride complex phase ceramic surface also there is not yet so far report.
Metal boride/Al
2O
3Pottery as high temperature complex phase ceramic and conventional ceramic phase than having high fusing point, high hardness, high thermal conductivity, wear resistance and high chemical stability.With metal boride/Al
2O
3Multiphase ceramic powder is filled in organic resin, can greatly improve thermotolerance and the wear resistance of organic resin.But, metal boride/Al
2O
3Still exist structure dissmilarity, the inconsistent problem in interface between multiphase ceramic powder and organic resin, serious restriction metal boride/Al
2O
3The high performance performance of complex phase powder in organic resin.Therefore, to metal boride/Al
2O
3The organic functional group modification is carried out to realizing the good compound very necessary of itself and organic resin in the multiphase ceramic powder surface.
Summary of the invention
The object of the invention is to by surperficial organic functional group modification, solve high-performance metal boride/Al
2O
3The problem that multiphase ceramic powder and organic resin interface compatibility are poor provides a kind of and organic resin to have good structural similarity, and interface compatibility good surface is through the high performance metal boride/Al of organic functional group chemical bonding modification
2O
3Multiphase ceramic powder.
Metal boride/the Al of a kind of high performance surperficial organic functional group chemical bonding of preparation modification that the present invention proposes
2O
3Multiphase ceramic powder is characterized in that it comprises the steps:
1) with particle diameter less than 100 μ m metal boride/Al
2O
3Multiphase ceramic powder joins in the ethanol hydrolysis solution that contains the surface-modifying agent that has organic functional group in a certain amount of structure, presses metal boride/Al
2O
3The complex phase powder: ethanol hydrolysis solution=1 gram: the ratio of 5 ~ 10 milliliters adds; Wherein, in ethanol hydrolysis solution, the ratio of surface-modifying agent and aqueous ethanolic solution is 1 gram: 50 milliliters, the ratio of ethanol and water is 1:9 (volume ratio); Reaction constant temperature is in 40 ~ 50 ℃, mechanical stirring 1 ~ 2 hour, ultra-sonic dispersion number minute; Obtain the surface through the boride/Al of organic functional group chemical bonding modification
2O
3The multiphase ceramic powder slip;
2) the complex phase powder slip that step 1) is obtained is by centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, get product.
Described metal boride is one or more in TiB2, zirconium diboride, two chromium borides or hafnium boride.
Described surface-modifying agent is take silane coupling agent, titanate coupling agent, aluminate coupling agent or bimetal coupling agent as best.
The present invention is with metal boride/Al
2O
3Multiphase ceramic powder carries out surperficial organic functional group chemical bonding modification, prepares the surface and has metal boride/Al by the organic functional group of chemical bond joining
2O
3Composite granule.Surface-modifying agent used in the present invention is coupling agent.The maximum characteristics of coupling agent molecule structure are to contain two different groups of chemical property in molecule, and one is the group of close inorganics, are easy to inorganics surface generation chemical reaction; Another is close organic group, can or generate hydrogen bond with organic resin generation chemical reaction and be dissolved in wherein.By close inorganics group and the metal boride/Al in the coupling agent structure
2O
3Hydroxyl reaction occurs in the multiphase ceramic powder surface, makes the close organism group in the coupling agent structure be connected to the complex phase powder surface by chemical reaction, realizes metal boride/Al
2O
3The organic functional modification of multiphase ceramic powder surface.The composite granule of surface organic modification is because organic group is contained on the surface, makes the interface compatibility of itself and organic resin be greatly improved.The organic resin of comparing its filling of ceramic powder provided by the present invention with conventional ceramic powder has higher thermotolerance and wear resisting property.
The preparation technology of composite granule of the present invention is simple, and is easy to operate, given surface organic modification boride/Al
2O
3The character such as the kind of composite granule organic functional group, concentration can be easy to control by regulating concentration and the temperature of reaction of coupling agent structure species, coupling agent ethanol hydrolysis solution, and low cost of manufacture is suitable for large-scale industrial production.Fig. 2 and Fig. 3 are respectively metal boride/Al
2O
3The stereoscan photograph of complex phase powder surface before and after the modification of coupling agent chemical bonding can be found out, the complex phase powder surface because of the introducing of organic group, and makes pitch smaller between powder granule after the organic coupling agent modification.Fig. 4 and Fig. 5 are respectively metal boride/Al
2O
3The complex phase powder surface is through the infrared spectra spectrogram of coupling agent modified front and back.Analysis of spectra learns that the complex phase powder surface after modification has been introduced organic group, and is that mode with chemical bond is connected between organic group and complex phase powder, illustrates under certain conditions, at metal boride/Al
2O
3The complex phase powder surface is can obtain the surface to connect the metal boride complex phase powder body material of organic functional group in the mode of chemical bonding by coupling agent modified processing.
Description of drawings
The preparation flow figure of Fig. 1 composite granule of the present invention.
Fig. 2 is metal boride/Al
2O
3Stereoscan photograph before the multiphase ceramic powder surface organic modification.
Fig. 3 is metal boride/Al
2O
3Stereoscan photograph after the multiphase ceramic powder surface organic modification.
Fig. 4 is metal boride/Al
2O
3Infrared spectra before the multiphase ceramic powder surface organic modification.
Fig. 5 is metal boride/Al
2O
3Infrared spectra after the multiphase ceramic powder surface organic modification.
Embodiment
5g silane coupling agent (titanate coupling agent, aluminate coupling agent, bimetal coupling agent) is joined in 250ml aqueous ethanolic solution (ethanol: water=1:9, volume ratio), stir hydrolysis.Then with 50g metal boride/Al
2O
3Multiphase ceramic powder joins in above-mentioned ethanol hydrolysis solution, mechanical stirring 1 ~ 2 hour, and ultra-sonic dispersion 10 minutes, temperature of reaction is controlled at 40 ~ 50 ℃.After reaction with uniform slip centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, obtain surperficial metal boride/Al through the modification of silane coupling agent chemical bonding
2O
3Multiphase ceramic powder.This complex phase powder has improved the similarity of inorganic powder and organic resin structure due to the introducing of organic group, has improved the interface compatibility of itself and organic resin.
Embodiment 2
8g titanate coupling agent (silane coupling agent, aluminate coupling agent, bimetal coupling agent) is joined in 400ml aqueous ethanolic solution (ethanol: water=1:9, volume ratio), stir hydrolysis.Then with 80g metal boride/Al
2O
3Multiphase ceramic powder joins in above-mentioned ethanol hydrolysis solution, mechanical stirring 1 ~ 2 hour, and ultra-sonic dispersion 10 minutes, temperature of reaction is controlled at 40 ~ 50 ℃.After reaction with uniform slip centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, obtain surperficial metal boride/Al through the modification of titanate coupling agent chemical bonding
2O
3Multiphase ceramic powder.This complex phase powder has improved the similarity of inorganic powder and organic resin structure due to the introducing of organic group, has improved the interface compatibility of itself and organic resin.
Embodiment 3
4g aluminate coupling agent (silane coupling agent, titanate coupling agent, bimetal coupling agent) is joined in 200ml aqueous ethanolic solution (ethanol: water=1:9, volume ratio), stir hydrolysis.Then with 40g metal boride/Al
2O
3Multiphase ceramic powder joins in above-mentioned ethanol hydrolysis solution, mechanical stirring 1 ~ 2 hour, and ultra-sonic dispersion 10 minutes, temperature of reaction is controlled at 40 ~ 50 ℃.After reaction with uniform slip centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, obtain surperficial metal boride/Al through the modification of aluminate coupling agent chemical bonding
2O
3Multiphase ceramic powder.This complex phase powder has improved the similarity of inorganic powder and organic resin structure due to the introducing of organic group, has improved the interface compatibility of itself and organic resin.
Embodiment 4
2g bimetal coupling agent (titanate coupling agent, aluminate coupling agent, silane coupling agent) is joined in 100ml aqueous ethanolic solution (ethanol: water=1:9, volume ratio), stir hydrolysis.Then with 20g metal boride/Al
2O
3Multiphase ceramic powder joins in above-mentioned ethanol hydrolysis solution, mechanical stirring 1 ~ 2 hour, and ultra-sonic dispersion 10 minutes, temperature of reaction is controlled at 40 ~ 50 ℃.After reaction with uniform slip centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, obtain surperficial metal boride/Al through the modification of bimetal coupling agent chemical bonding
2O
3Multiphase ceramic powder.This complex phase powder has improved the similarity of inorganic powder and organic resin structure due to the introducing of organic group, has improved the interface compatibility of itself and organic resin.
Embodiment 5
10g silane coupling agent (titanate coupling agent, aluminate coupling agent, bimetal coupling agent) is joined in 500ml aqueous ethanolic solution (ethanol: water=1:9, volume ratio), stir hydrolysis.Then with 100g metal boride/Al
2O
3Multiphase ceramic powder joins in above-mentioned ethanol hydrolysis solution, mechanical stirring 1 ~ 2 hour, and ultra-sonic dispersion 10 minutes, temperature of reaction is controlled at 40 ~ 50 ℃.After reaction with uniform slip centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, obtain surperficial metal boride/Al through the modification of silane coupling agent chemical bonding
2O
3Multiphase ceramic powder.This complex phase powder has improved the similarity of inorganic powder and organic resin structure due to the introducing of organic group, has improved the interface compatibility of itself and organic resin.
Claims (5)
1. the metal boride of a surface modification/aluminium sesquioxide multiphase ceramic powder, it is characterized in that being made of the organic functional group of metal boride/aluminium sesquioxide complex phase ceramic particle and particle surface.
2. the metal boride of surface modification according to claim 1/aluminium sesquioxide multiphase ceramic powder, is characterized in that, described particle surface organic functional group is to form by particle and surface-modifying agent generation chemical bonding.
3. according to claim 1, the metal boride of 2 described surface modifications/aluminium sesquioxide multiphase ceramic powder is characterized in that, described surface-modifying agent is silane coupling agent, titanate coupling agent, aluminate coupling agent or bimetal coupling agent.
4. the metal boride of surface modification according to claim 1/aluminium sesquioxide multiphase ceramic powder, is characterized in that, described metal boride is one or more in TiB2, zirconium diboride, two chromium borides or hafnium boride.
5. the preparation method of the metal boride of a surface modification as claimed in claim 1/aluminium sesquioxide multiphase ceramic powder is characterized in that concrete steps are as follows:
1) metal boride/aluminium sesquioxide multiphase ceramic powder is joined in the ethanol hydrolysis solution that contains the coupling agent that has organic functional group in a certain amount of structure, in metal boride/aluminium sesquioxide complex phase powder: ethanol hydrolysis solution=1 gram: the ratio of 5 ~ 10 milliliters adds; Wherein, in ethanol hydrolysis solution, the ratio of coupling agent and aqueous ethanolic solution is 1 gram: 50 milliliters, the volume ratio of ethanol and water is 1:9; Reaction constant temperature is in 40 ~ 50 ℃, mechanical stirring 1 ~ 2 hour, ultra-sonic dispersion number minute; Obtain surperficial boride through the modification of organic functional group chemical bonding/aluminium sesquioxide multiphase ceramic powder slip;
2) the complex phase powder slip that step 1) is obtained is by centrifugation, and with the powder that separates with after washing with acetone 2-3 time in the vacuum drying oven of 80 ℃ dry 12 hours, get product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI617533B (en) * | 2016-12-09 | 2018-03-11 | 財團法人工業技術研究院 | Surface-treated ceramic powder and applications thereof |
| CN111377735A (en) * | 2018-12-27 | 2020-07-07 | 上海元颉新材料科技有限公司 | Surface-modified nano zirconia ceramic powder and preparation method and application thereof |
| CN116759706A (en) * | 2023-07-17 | 2023-09-15 | 广东中宇恒通电热科技有限公司 | High-temperature-resistant high-humidity safe heating film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182191A (en) * | 2007-11-15 | 2008-05-21 | 复旦大学 | Method for preparing rear-earth modified zirconium diboride/aluminum oxide composite powder |
| CN102660154A (en) * | 2012-04-28 | 2012-09-12 | 常州大学 | Surface modification method for nanometer titanium dioxide |
-
2013
- 2013-03-13 CN CN2013100787309A patent/CN103160148A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182191A (en) * | 2007-11-15 | 2008-05-21 | 复旦大学 | Method for preparing rear-earth modified zirconium diboride/aluminum oxide composite powder |
| CN102660154A (en) * | 2012-04-28 | 2012-09-12 | 常州大学 | Surface modification method for nanometer titanium dioxide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI617533B (en) * | 2016-12-09 | 2018-03-11 | 財團法人工業技術研究院 | Surface-treated ceramic powder and applications thereof |
| US10894288B2 (en) | 2016-12-09 | 2021-01-19 | Industrial Technology Research Institute | Surface-treated ceramic powder and applications thereof |
| CN111377735A (en) * | 2018-12-27 | 2020-07-07 | 上海元颉新材料科技有限公司 | Surface-modified nano zirconia ceramic powder and preparation method and application thereof |
| CN116759706A (en) * | 2023-07-17 | 2023-09-15 | 广东中宇恒通电热科技有限公司 | High-temperature-resistant high-humidity safe heating film |
| CN116759706B (en) * | 2023-07-17 | 2024-01-02 | 广东中宇恒通电热科技有限公司 | High-temperature-resistant high-humidity safe heating film |
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Application publication date: 20130619 |