CN106608712A - In-situ reaction whisker glass ceramic and preparation method thereof - Google Patents
In-situ reaction whisker glass ceramic and preparation method thereof Download PDFInfo
- Publication number
- CN106608712A CN106608712A CN201510681246.4A CN201510681246A CN106608712A CN 106608712 A CN106608712 A CN 106608712A CN 201510681246 A CN201510681246 A CN 201510681246A CN 106608712 A CN106608712 A CN 106608712A
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- devitrified glass
- glass ceramic
- raw material
- situ preparation
- whisker
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/06—Whiskers ss
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses an in-situ reaction whisker glass ceramic and a preparation method thereof. Chemical compositions of a glass ceramic raw meal comprise, by mass, 60-90 parts of glass raw material, 1-10 parts of nucleating agent and 5-20 parts of metal powder, wherein chemical compositions of the glass raw material comprise, by mass, 30-60 parts of SiO2, 20-50 parts of Al2O3, 1-10 parts of B2O3, 1-10 parts of K2O, and 1-10 parts of Na2O; the nucleating agent is one of MnO2, TiO2 and ZrO2; the metal powder is aluminum powder or copper powder. The preparation method comprises the steps that mixing is conducted according to the compositions of the glass raw material, firing is conducted at the temperature ranging from 1200 DEG C to 1500 DEG C for 120-240 min, water quenching is conducted, and a glass ceramic precursor is obtained; the glass ceramic precursor, the nucleating agent and the metal powder are mixed and are subjected to ball milling to obtain the glass ceramic raw meal; the glass ceramic raw meal is loaded into a mold and is subjected to dry pressing to prepare a glass ceramic green body, and the glass ceramic green body is subjected to thermal treatment at the temperature ranging from 650 DEG C to 850 DEG C to obtain the in-situ reaction whisker glass ceramic. In the glass ceramic, whiskers are generated in situ in a glass ceramic matrix; the preparation process is simple; the whiskers in the glass ceramic matrix are dispersed uniformly; the combination of the whiskers and the glass ceramic matrix is good; and the mechanical properties of the glass ceramic are improved.
Description
Technical field
The invention belongs to devitrified glass art field, more particularly to a kind of devitrified glass of in-situ preparation whisker and preparation method thereof.
Background technology
Devitrified glass is widely used in the fields such as space flight, machinery, building, medical treatment because the coefficient of expansion is adjustable, chemical stability is good, heat endurance is good, using temperature is high and hard wear resistant as a kind of Inorganic Non-metallic Materials of excellent performance.Crystal whisker toughened devitrified glass can significantly improve devitrified glass fragility, further improve devitrified glass mechanical property, widen the use range of devitrified glass.The method that the doping whisker for using at present prepares crystal whisker toughened devitrified glass, there is preparation process complex process, whisker disperses inequality in devitrified glass, the problems such as whisker is combined insecure with matrix, it is therefore necessary to the preparation method for obtaining the crystal whisker toughened devitrified glass of in-situ preparation and the formula for developing suitable devitrified glass.
The content of the invention
For above-mentioned the deficiencies in the prior art, the invention provides a kind of devitrified glass of in-situ preparation whisker, by the crystal whisker toughened devitrified glass of in-situ preparation, improve devitrified glass intensity and evade the whisker dispersion inequality produced during additional crystal whisker toughened devitrified glass simultaneously, whisker combined with matrix it is insecure, the problems such as complex process.
The technical scheme is that：
A kind of devitrified glass of the in-situ preparation whisker, it is characterised in that：The mass fraction of devitrified glass raw material chemical composition is：Frit：60 ~ 90, nucleating agent：1 ~ 10, metal powder：5~20.
Further prioritization scheme, a kind of devitrified glass of in-situ preparation whisker, it is characterised in that：The mass fraction of the chemical composition of frit is：SiO2：30 ~ 60, Al2O3：20 ~ 50, B2O3：1 ~ 10, K2O：1~10 Na2O：1~10.
Further prioritization scheme, a kind of devitrified glass of in-situ preparation whisker, it is characterised in that：Nucleating agent is MnO2、ZrO2And TiO2In one kind.
Further prioritization scheme, a kind of devitrified glass of in-situ preparation whisker, it is characterised in that：Metal powder is aluminium powder or copper powder.
A kind of preparation method for preparing in-situ preparation devitrified glass, it is characterised in that：The method is comprised the following steps：
Step 1：Proportioning according to frit weighs frit raw material, and is well mixed, and 1200 DEG C ~ 1500 DEG C of high temperature is fired 120 ~ 240 minutes, is then carried out water quenching and is obtained devitrified glass presoma；
Step 2：The devitrified glass presoma that water quenching in step 1 is obtained is well mixed with nucleating agent, metal powder with ball mill, obtains devitrified glass raw material；
Step 3：The devitrified glass raw material obtained in step 2 are fitted into into dry-pressing in mould and prepare devitrified glass raw material base substrate；
Step 4：Devitrified glass raw material base substrate obtained by step 3 is put in 650 DEG C ~ 850 DEG C of Muffle furnace, along with the furnace cooling after 1 ~ 2h of heat treatment, i.e., in the devitrified glass for obtaining in-situ preparation whisker.
Further prioritization scheme, a kind of preparation method of the devitrified glass for preparing in-situ preparation whisker, it is characterised in that：The frit stated used, the quality purity of nucleating agent are not less than 99.9% in step 1, step 2.
Further prioritization scheme, a kind of preparation method of the devitrified glass for preparing in-situ preparation whisker, it is characterised in that：Drum's speed of rotation described in step 2 is 300 ~ 450 revs/min, and the time is 4h.
Further prioritization scheme, a kind of preparation method of the devitrified glass for preparing in-situ preparation whisker, it is characterised in that：Dry-pressing formed pressure is 30 ~ 45Mpa, time 10min in step 3.
Beneficial effects of the present invention
The result of the present invention shows, using the devitrified glass of the generated in-situ whisker of present invention preparation, because whisker is generated in glass basis situ, preparation process is simple, whisker is uniformly dispersed in glass basis, and whisker is well combined with glass basis, improves the mechanical property of devitrified glass.
Description of the drawings
Fig. 1 be the present invention prepare in-situ preparation whisker devitrified glass the plane of disruption in whisker electron scanning micrograph.
Specific embodiment
The making of the frit of embodiment 1
The material for providing the primary chemical composition of frit is respectively silica, alundum (Al2O3), boric acid, potassium hydroxide, NaOH.The mass fraction of each material is after by calculating conversion：Silica：37.30, alundum (Al2O3)：32.15, boric acid：13.48, potassium hydroxide：10.03, NaOH：7.04.The amount of each material is weighed according to the above ratio.
Manufacturing process：Above-mentioned raw materials are well mixed, the scorification in the environment of 1500 DEG C, water-filling of going forward side by side is quenched and obtains devitrified glass presoma.
The making of the devitrified glass raw material of embodiment 2
According to mass fraction：Devitrified glass presoma：80, manganese dioxide：8, aluminium powder：12 weigh respective substance, are put into ball milling in ball mill and obtain devitrified glass raw material in four hours.
The making of the devitrified glass raw material base substrate of embodiment 3
The devitrified glass raw material prepared in embodiment 1 are fitted in mould, keep 10min, the dry-pressing formed rear demoulding to obtain devitrified glass raw material base substrate under 35Mpa pressure.
The making of the devitrified glass of the in-situ preparation whisker of embodiment 4
Devitrified glass raw material base substrate in embodiment 3 is dried into 60 ~ 120min in 60 ~ 100 DEG C of environment, along with the furnace cooling after 1 ~ 2h is then heat-treated in 650 DEG C ~ 850 DEG C of environment, i.e., in the devitrified glass for obtaining in-situ preparation whisker.
Claims (8)
1. a kind of devitrified glass of in-situ preparation whisker, it is characterised in that：The mass fraction of devitrified glass raw material chemical composition is：Frit：60 ~ 90, nucleating agent：1 ~ 10, metal powder：5~20.
2. a kind of devitrified glass of in-situ preparation whisker according to claim 1, it is characterised in that：The mass fraction of the chemical composition of frit is：SiO2：30 ~ 60, Al2O3：20 ~ 50, B2O3：1 ~ 10, K2O：1~10 Na2O：1~10.
3. a kind of devitrified glass of in-situ preparation whisker according to claim 1, it is characterised in that：Nucleating agent is MnO2、ZrO2And TiO2In one kind.
4. a kind of devitrified glass of in-situ preparation whisker according to claim 1, it is characterised in that：Metal powder is aluminium powder or copper powder.
5. the method that one kind prepares the devitrified glass of in-situ preparation whisker described in claim 1 ~ 4, it is characterised in that：The method is comprised the following steps：
Step 1：Proportioning according to frit weighs frit raw material, and is well mixed, and 1200 DEG C ~ 1500 DEG C of high temperature is fired 120 ~ 240 minutes, is then carried out water quenching and is obtained devitrified glass presoma；
Step 2：The devitrified glass presoma that water quenching in step 1 is obtained is well mixed with nucleating agent, metal powder with ball mill, obtains devitrified glass raw material；
Step 3：The devitrified glass raw material obtained in step 2 are fitted into into dry-pressing in mould and prepare devitrified glass raw material base substrate；
Step 4：Devitrified glass raw material base substrate obtained by step 3 is put in 650 DEG C ~ 850 DEG C of Muffle furnace, along with the furnace cooling after 1 ~ 2h of heat treatment, i.e., in the devitrified glass for obtaining in-situ preparation whisker.
6. a kind of method of the devitrified glass for preparing in-situ preparation whisker according to claim 5, it is characterised in that：The quality purity of frit, nucleating agent described in step 1, step 2 is not less than 99.9%.
7. a kind of method of the devitrified glass for preparing in-situ preparation whisker according to claim 5, it is characterised in that：Drum's speed of rotation described in step 2 is 300 ~ 450 revs/min, and the time is 4h.
8. a kind of method of the devitrified glass for preparing in-situ preparation whisker according to claim 5, it is characterised in that：Dry-pressing formed pressure is 30 ~ 45Mpa, time 10min in step 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510681246.4A CN106608712A (en) | 2015-10-21 | 2015-10-21 | In-situ reaction whisker glass ceramic and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510681246.4A CN106608712A (en) | 2015-10-21 | 2015-10-21 | In-situ reaction whisker glass ceramic and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN106608712A true CN106608712A (en) | 2017-05-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510681246.4A Pending CN106608712A (en) | 2015-10-21 | 2015-10-21 | In-situ reaction whisker glass ceramic and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585528A (en) * | 2018-05-17 | 2018-09-28 | 天长市天意玻璃制品有限公司 | A kind of novel nucleated glass and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5186729A (en) * | 1991-04-26 | 1993-02-16 | Center For Innovative Technology | Method of making in-situ whisker reinforced glass ceramic |
| CN1433980A (en) * | 2003-03-01 | 2003-08-06 | 大连理工大学 | Method for making composite type nucleated glass from flyash used in building |
| CN104529167A (en) * | 2015-01-07 | 2015-04-22 | 中南大学 | In-situ growth beta-Si3N4 fiber/rod-like crystal enhanced glass-ceramic composite material and preparation method thereof |
-
2015
- 2015-10-21 CN CN201510681246.4A patent/CN106608712A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5186729A (en) * | 1991-04-26 | 1993-02-16 | Center For Innovative Technology | Method of making in-situ whisker reinforced glass ceramic |
| CN1433980A (en) * | 2003-03-01 | 2003-08-06 | 大连理工大学 | Method for making composite type nucleated glass from flyash used in building |
| CN104529167A (en) * | 2015-01-07 | 2015-04-22 | 中南大学 | In-situ growth beta-Si3N4 fiber/rod-like crystal enhanced glass-ceramic composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 中国航空工业集团公司复合材料技术中心主编: "《航空复合材料》", 31 December 2013, 北京：航空工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585528A (en) * | 2018-05-17 | 2018-09-28 | 天长市天意玻璃制品有限公司 | A kind of novel nucleated glass and preparation method thereof |
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