CN106630987A - Oxide catalyst for preparation of mullite ceramic whiskers - Google Patents
Oxide catalyst for preparation of mullite ceramic whiskers Download PDFInfo
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- CN106630987A CN106630987A CN201610829195.XA CN201610829195A CN106630987A CN 106630987 A CN106630987 A CN 106630987A CN 201610829195 A CN201610829195 A CN 201610829195A CN 106630987 A CN106630987 A CN 106630987A
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- mullite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the field of catalysts and ceramic whiskers and discloses a novel oxide catalyst for preparation of mullite (3Al2O3.2SiO2) ceramic whiskers. The oxide catalyst for promoting growth of the mullite ceramic whiskers is MoO3 or (NH4)2MoO4, and in application of the MoO3 or (NH4)2MoO4 as the catalyst for promoting growth of the mullite ceramic whiskers, a mole ratio of the catalyst to mullite is controlled to be 0-1, namely (3Al2O3.2SiO2)1-x(MoO3)x, wherein x refers to 0-0.5. By adoption of a solid phase method or a liquid phase method for synthesis of the mullite whiskers, the mullite whiskers uniform in morphology, 1-10micron in length range and 5-20 in length-diameter ratio range can be acquired through regulation of catalyst content and sintering temperature. By adoption of the catalyst for preparation of the mullite ceramic whiskers, low synthesis temperature, whisker morphologic uniformity, large length-diameter ratio, simplicity in preparation process, high reaction degree, freeness of aluminum oxide and quartz phase of prepared mullite and the like are realized.
Description
Technical field
The invention belongs to catalyst field, discloses a kind of oxide catalyst prepared for mullite crystal whisker.
Background technology
Ceramic whisker is a kind of important structural material.The composite of whisker reinforcement in mechanical property (such as：Fracture is tough
Property, bending strength, thermal shock resistance etc.) on can be greatly improved.The crystal whisker materials such as carborundum, silicon nitride and potassium titanate are
It is widely used in the preparation of excellent performance composite.However, the easy oxidation Decomposition of these crystal whisker materials at high temperature, causes machine
Tool property fails.Mullite material is Al2O3-SiO2Unique stable crystalline material in system, due to high mechanical strength,
Good creep-resistant property, low thermal coefficient of expansion, good chemical and high-temperature stability, has become the time of advanced configuration material
Choosing.Mullite crystal is more than other directions in the crystallography c-axis direction speed of growth, is easily-synthesized one-dimensional crystal whisker materials.Mullite is made pottery
The composite of porcelain whisker reinforcement has begun to be taken seriously.
Many methods are used for mullite synthesizing whisker, such as solid reaction process, sol-gal process, coprecipitation.However, sharp
With these methods in relatively low synthesis temperature, prepare that pattern is good, the mullite crystal whisker that draw ratio is big need to add it is appropriate
Catalyst.Generally AlF3It is mullite crystal whisker growth catalyst that everybody commonly uses.Additionally, there is some oxide catalysts
Such as La2O3,Co2O3Deng, but effect is not as good as AlF3.Here, it has been found that a kind of new oxide catalyst, molybdenum oxide (or
Ammonium molybdate), show good mullite crystal whisker growth catalytic action.
The content of the invention
It is an object of the invention to provide a kind of oxide catalyst --- molybdenum oxide prepared for mullite ceramic whisker
(or ammonium molybdate), using this catalyst mullitization temperature can be effectively reduced, and improve the mullitization extent of reaction, prepare pattern
The big mullite ceramic whisker of homogeneous, draw ratio.
Using molybdenum oxide by solid reaction process mullite synthesizing ceramic whisker, comprise the following steps：
(1) by chemical formula (3Al2O3·2SiO2)1-x(MoO3)x(x=0-0.5) catalysis of silicon source, silicon source and molybdenum oxide is carried out
The synthesis materials such as agent are weighed；
(2) anhydrous ethanol solvent and zirconia ball mill are added in the synthesis material for weighing up, ball mill is placed in and is fully ground
Mill mixing；
(3) mixed uniformly powder material after grinding is placed in into 100 DEG C of dryings in baking oven, then the 1200- in Muffle furnace
1500 DEG C of high-temperature calcinations 2 hours, obtain mullite ceramic whisker.
Using ammonium molybdate by liquid phase reactor method mullite synthesizing ceramic whisker, comprise the following steps：
(1) according to chemical formula (3Al2O3·2SiO2)1-x(MoO3)x(x=0-0.5) tetraethyl orthosilicate (TEOS) is measured, is claimed
Take aluminium chloride and ammonium molybdate catalyst；
(2) TEOS is dissolved in into ethanol and is configured to the solution that concentration is 1mol/L, and pH value is adjusted to 2 with hydrochloric acid；By aluminium chloride
Water is dissolved in ammonium molybdate, the solution that concentration of aluminum chloride is 0.5mol/L is configured to；
(3) above two solution is mixed and is incorporated in 60 DEG C of heating stirrings, 200 DEG C of roastings in baking oven are transferred to after gelling；Will
Powder after roasting is placed in Muffle furnace 1200-1500 DEG C of high-temperature calcination 2 hours, obtains mullite ceramic whisker.
For two kinds of mullite ceramic whisker synthesis methods, can respectively adjust catalyst content and calcining heat optimization does not come
Prepared by the synthesis condition of feldspar whisker, the regulation and control for realizing mullite ceramic whisker, obtain optimum mullite crystal whisker material.
The present invention has the beneficial effect that to mullite synthesis：
(1) using this catalyst mullitization temperature can be caused effectively to reduce, course of reaction simplifies.For example, kaolin/hydrogen
Alumina system, using molybdenum oxide catalyst solid phase reaction mullite crystal whisker is prepared, and mullitization temperature reduces by 200 DEG C, reaction
Process substantially simplifies.(see accompanying drawing 1)
(2) the system mullitization extent of reaction can be increased using this catalyst, prepared mullite is not salic
With quartzy phase.(see accompanying drawing 1)
(3) the mullite ceramic whisker that pattern is homogeneous, draw ratio is big can be prepared using this catalyst.(see accompanying drawing 2)
(4) it is capable of achieving the regulation and control preparation of mullite ceramic whisker by changing catalyst and calcining heat.
Description of the drawings
Impact of Fig. 1 molybdenum oxides to kaolin/aluminium hydroxide system mullite building-up process.The XRD of (a) containing molybdenum oxide
Figure；The XRD of (b) without molybdenum oxide.Mullite is 4 with the mol ratio of catalyst:1
The mullite ceramic whisker microstructure that Fig. 2 is synthesized using kaolin, aluminium hydroxide and molybdenum oxide catalyst.Mo Lai
Stone is 4 with the mol ratio of catalyst:1
The mullite crystal whisker that Fig. 3 is synthesized using kaolin, aluminium hydroxide and molybdenum oxide catalyst under different calcining heats
Size.Mullite is 4 with the mol ratio of catalyst:1
Specific embodiment
Case study on implementation 1：Kaolin/aluminium hydroxide system adds molybdenum oxide solid phase reaction to prepare mullite crystal whisker
By chemical formula (3Al2O3·2SiO2)0.8(MoO3)0.2, quantitatively weigh kaolin, aluminium hydroxide and molybdenum oxide；To claim
Measured powder inserts ball milling bottle, adds absolute ethyl alcohol and zirconia ball mill that mixing is fully ground on ball mill；Will grinding
Afterwards uniform mixed powder is placed in 100 DEG C of dryings of baking oven, and then 1200-1500 DEG C of high-temperature calcination 2 hours in Muffle furnace, obtain not
Carry out feldspar whisker.
Fig. 1 is the X ray diffracting spectrum of different temperatures calcining sample in the present embodiment, the visible addition molybdenum oxide of Comparative map
Afterwards, mullitization temperature is reduced, and course of reaction substantially simplifies.
Fig. 2 is the SEM patterns of the mullite crystal whisker prepared under different calcining heats in the present embodiment.Known by figure, it is made
Standby whisker morphology is homogeneous, and, in 500nm or so, length is in 1-10 micrometer ranges for width.Calcining heat can be with more than 1300 DEG C
Obtain the mullite ceramic whisker that pattern is good and homogeneous, draw ratio is big.
Fig. 3 is the mullite crystal whisker size prepared under different calcining heats in the present embodiment.Known by figure, raised with temperature,
Width is almost unchanged, and length constantly increases, and draw ratio increases to 20 by 5.
Case study on implementation 2：Quartz/aluminium hydroxide system adds molybdenum oxide solid phase reaction to prepare mullite crystal whisker
By chemical formula (3Al2O3·2SiO2)0.8(MoO3)0.2, quantitatively weigh silica flour, aluminium hydroxide and molybdenum oxide；To claim
Measured powder inserts ball milling bottle, adds absolute ethyl alcohol and zirconia ball mill that mixing is fully ground on ball mill；Will grinding
Afterwards uniform mixed powder is placed in 100 DEG C of dryings of baking oven, and then 1300-1500 DEG C of high-temperature calcination 2 hours in Muffle furnace, obtain not
Carry out feldspar whisker.
Case study on implementation 3：Silicon powder/aluminium hydroxide system adds molybdenum oxide solid phase reaction to prepare mullite crystal whisker
By chemical formula (3Al2O3·2SiO2)0.8(MoO3)0.2, quantitatively weigh silicon powder, aluminium hydroxide and molybdenum oxide；To claim
Measured powder inserts ball milling bottle, adds absolute ethyl alcohol and zirconia ball mill that mixing is fully ground on ball mill；Will grinding
Afterwards uniform mixed powder is placed in 100 DEG C of dryings of baking oven, and then 1300-1500 DEG C of high-temperature calcination 2 hours in Muffle furnace, obtain not
Carry out feldspar whisker.
Case study on implementation 4：Aluminium chloride/TEOS systems add ammonium molybdate to prepare mullite crystal whisker
According to chemical formula (3Al2O3·2SiO2)0.8(MoO3)0.2Tetraethyl orthosilicate (TEOS) is measured, aluminium chloride and molybdenum is weighed
Sour ammonium catalyst；TEOS is dissolved in into ethanol and is configured to the solution that concentration is 1mol/L, and pH value is adjusted to 2 with hydrochloric acid；By aluminium chloride
Water is dissolved in ammonium molybdate, the solution that concentration of aluminum chloride is 0.5mol/L is configured to；By above two solution it is mixed be incorporated in 60 DEG C plus
Thermal agitation, is transferred to 200 DEG C of roastings in baking oven after gelling；Powder after roasting is placed in into 1300-1500 DEG C of high temperature in Muffle furnace
Calcining 2 hours, obtains mullite ceramic whisker.
Described above, only using the embodiment of this origination techniques content, any those skilled in the art are with this wound
Make done modification, change, all belong to the scope of the claims of this creation opinion, and be not limited to those disclosed embodiments.
Claims (5)
1. a kind of oxide catalyst prepared for mullite ceramic whisker, is molybdenum oxide (or ammonium molybdate), and chemical formula is MoO3
(or (NH4)2MoO4).Using the mol ratio of the catalyst preparation mullite ceramic whisker, catalyst and mullite in 0-1 scopes
It is advisable, i.e. (3Al2O3·2SiO2)1-x(MoO3)x, x=0-0.5.
2. according to claim 1, mullite ceramic whisker is prepared using solid reaction process, it is characterised in that including following
Step：
(1) by chemical formula (3Al2O3·2SiO2)1-x(MoO3)x(x=0-0.5) silicon source, silicon source and molybdenum oxide catalyst etc. are carried out
Synthesis material is weighed；
(2) anhydrous ethanol solvent and zirconia ball mill are added in the synthesis material for weighing up, be placed in ball mill be fully ground it is mixed
Close；
(3) mixed uniformly powder material after grinding is placed in into 100 DEG C of dryings in baking oven, then the 1200-1500 in Muffle furnace
DEG C high-temperature calcination 2 hours, obtains mullite ceramic whisker.
3. according to claim 1, mullite ceramic whisker is prepared using liquid phase reactor method (sol-gel process), its feature
It is to comprise the following steps：
(1) according to chemical formula (3Al2O3·2SiO2)1-x(MoO3)x(x=0-0.5) tetraethyl orthosilicate (TEOS) is measured, chlorine is weighed
Change aluminium and ammonium molybdate catalyst；
(2) TEOS is dissolved in into ethanol and is configured to the solution that concentration is 1mol/L, and pH value is adjusted to 2 with hydrochloric acid；By aluminium chloride and molybdenum
Sour ammonium is dissolved in water, is configured to the solution that concentration of aluminum chloride is 0.5mol/L；
(3) above two solution is mixed and is incorporated in 60 DEG C of heating stirrings, 200 DEG C of roastings in baking oven are transferred to after gelling；By roasting
Powder afterwards is placed in Muffle furnace 1200-1500 DEG C of high-temperature calcination 2 hours, obtains mullite ceramic whisker.
4. according to claims 1,2 and 3, different material system can be obtained by optimization calcining heat and catalyst content
Mullite crystal whisker calcining heat that must be optimum and catalyst content.
5. mullite ceramic whisker is prepared according to claim 1,2,3 and 4, it is characterised in that：Synthesis temperature is low, whisker shape
Looks are homogeneous, draw ratio is big, and preparation process is simple, and the extent of reaction is high, the not salic and quartzy equal spy of prepared mullite
Point.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240483A (en) * | 2018-03-07 | 2019-09-17 | 海南大学 | A method of carborundum porous ceramics are prepared using crystal silicon waste mortar |
| CN110550965A (en) * | 2019-09-20 | 2019-12-10 | 中国民航大学 | Preparation method of mullite whisker low-temperature growth toughening type aluminum phosphate-based high-temperature adhesive |
| CN112456962A (en) * | 2019-09-09 | 2021-03-09 | 天津大学 | Fluorine-free preparation method of mullite fiber whisker reinforcement and aerogel prepared by fluorine-free preparation method |
| CN114933485A (en) * | 2022-06-30 | 2022-08-23 | 萍乡学院 | Whisker/fiber reinforced cordierite porous ceramic and preparation method and application thereof |
| CN116283238A (en) * | 2023-02-27 | 2023-06-23 | 萍乡学院 | Ceramic membrane for oil-water separation and preparation method thereof |
| CN116730707A (en) * | 2023-07-10 | 2023-09-12 | 广州华越新材料科技有限公司 | Long-acting antibacterial domestic ceramic and preparation method and application thereof |
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| CN1587450A (en) * | 2004-07-02 | 2005-03-02 | 北京理工大学 | Method for preparing mullite single crystal nano belt |
| WO2007045003A1 (en) * | 2005-10-21 | 2007-04-26 | Miba Sinter Austria Gmbh | Component, especially a preform, comprising a coating |
| CN101498049A (en) * | 2009-01-21 | 2009-08-05 | 景德镇陶瓷学院 | Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process |
| CN101935877A (en) * | 2010-09-03 | 2011-01-05 | 昆明理工大学 | Method for synthesizing mullite whiskers by normal pressure sintering |
| CN104130019A (en) * | 2014-07-10 | 2014-11-05 | 陕西科技大学 | Preparation method of carbon/carbon composite material mullite whisker toughened C-AlPO4-MoSi2 composite coating |
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|---|---|---|---|---|
| CN1587450A (en) * | 2004-07-02 | 2005-03-02 | 北京理工大学 | Method for preparing mullite single crystal nano belt |
| WO2007045003A1 (en) * | 2005-10-21 | 2007-04-26 | Miba Sinter Austria Gmbh | Component, especially a preform, comprising a coating |
| CN101498049A (en) * | 2009-01-21 | 2009-08-05 | 景德镇陶瓷学院 | Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process |
| CN101935877A (en) * | 2010-09-03 | 2011-01-05 | 昆明理工大学 | Method for synthesizing mullite whiskers by normal pressure sintering |
| CN104130019A (en) * | 2014-07-10 | 2014-11-05 | 陕西科技大学 | Preparation method of carbon/carbon composite material mullite whisker toughened C-AlPO4-MoSi2 composite coating |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240483A (en) * | 2018-03-07 | 2019-09-17 | 海南大学 | A method of carborundum porous ceramics are prepared using crystal silicon waste mortar |
| CN110240483B (en) * | 2018-03-07 | 2021-10-19 | 海南大学 | Method for preparing silicon carbide porous ceramic by using crystalline silicon waste mortar |
| CN112456962A (en) * | 2019-09-09 | 2021-03-09 | 天津大学 | Fluorine-free preparation method of mullite fiber whisker reinforcement and aerogel prepared by fluorine-free preparation method |
| CN110550965A (en) * | 2019-09-20 | 2019-12-10 | 中国民航大学 | Preparation method of mullite whisker low-temperature growth toughening type aluminum phosphate-based high-temperature adhesive |
| CN110550965B (en) * | 2019-09-20 | 2021-12-10 | 中国民航大学 | Preparation method of mullite whisker low-temperature growth toughening type aluminum phosphate-based high-temperature adhesive |
| CN114933485A (en) * | 2022-06-30 | 2022-08-23 | 萍乡学院 | Whisker/fiber reinforced cordierite porous ceramic and preparation method and application thereof |
| CN116283238A (en) * | 2023-02-27 | 2023-06-23 | 萍乡学院 | Ceramic membrane for oil-water separation and preparation method thereof |
| CN116730707A (en) * | 2023-07-10 | 2023-09-12 | 广州华越新材料科技有限公司 | Long-acting antibacterial domestic ceramic and preparation method and application thereof |
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