CN108947493A - A kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness - Google Patents

A kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness Download PDF

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CN108947493A
CN108947493A CN201810901429.6A CN201810901429A CN108947493A CN 108947493 A CN108947493 A CN 108947493A CN 201810901429 A CN201810901429 A CN 201810901429A CN 108947493 A CN108947493 A CN 108947493A
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temperature
based ceramics
nano oxidized
oxidized magnesium
nano
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莫云泽
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SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY Co Ltd
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SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a kind of preparation methods of the nano oxidized magnesium-based ceramics of high-compactness.The nano oxidized magnesium-based ceramics use high-purity nano magnesia for raw material, zirconium oxide, yttrium oxide, aluminium oxide and the titanium dioxide of high-purity are mixed into additive and are prepared, wherein content of magnesia >=85wt%, relative density >=95%, additive level 15wt%.The nano oxidized magnesium-based ceramics are prepared by the technique that liquid phase grinds mixing, spray drying granulation integration, high-pressure molding and high temperature sintering.Nano oxidized magnesium-based ceramics of the invention have the characteristics that consistency height, purity is high, high temperature resistant, corrosion-resistant, can prolonged application in environment such as the high temperature such as high-temperature calcination, metal smelt, highly corrosives, the stable preparation process, high yield rate, wide adaptation range are suitable for mass production.

Description

A kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness
Technical field
The invention belongs to the preparation technical fields of functional material, concretely relate to a kind of high-compactness nano magnesia The preparation method of base ceramics.
Background technique
Magnesium oxide-based ceramics belong to cubic system using magnesia as the ceramics of principal component, tensile strength, compression strength and anti- Curved intensity is all more much lower than sintered alumina, its elevated temperature strength is relatively low.Magnesia is good insulating body, at room temperature resistance Rate is increased with temperature, and resistivity drastically reduces.Magnesia ceramics is also typical basic refractory, in oxidizing atmosphere or nitrogen Protection under can steady operation to 2400 DEG C.Magnesia ceramics also acts as the crucible of metal smelting, also fits in atomic energy industry In the uranium and thorium of smelting high-purity；Also act as thermocouple protective casing.Using the property that it can be such that electromagnetic wave passes through, make radar Cover and the transmission window material of infra-red radiation etc..
High purity magnesium oxide ceramics have many advantages, such as high temperature resistant, corrosion-resistant, but high purity magnesium oxide ceramics are more difficult fine and close burns Knot is raw material using high-purity nano magnesia, since its bulk density is low, reactivity is strong so that powder processed, form it is certain Difficulty, especially prepare high-compactness large scale magnesia tube, crucible is easy to produce deformation, cracking phenomena such as.
This patent uses high-purity nano magnesia for raw material, zirconium oxide, yttrium oxide, aluminium oxide and the dioxy of high-purity Change titanium is mixed into additive and is prepared.Mixing, spray drying granulation integration, high-pressure molding and high temperature is ground by liquid phase to burn The nano oxidized magnesium-based ceramics are prepared in the technique of knot.It is uniform in mixing process that this method greatly improves raw material Degree, while dry and granulation is reduced to a step, it is greatly improved the quality of magnesium oxide-based ceramics.
Summary of the invention
It is an object of the invention to overcome low quality existing for the magnesium oxide-based ceramics of prior art preparation, mixing it is uneven, The low problem of yield rate provides a kind of preparation method with the stable nano oxidized magnesium-based ceramics of high-compactness.
To reach above-mentioned expected purpose, the present invention adopts the following technical scheme:
A kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness, which is characterized in that use high-purity nano magnesia for Raw material, zirconium oxide, yttrium oxide, aluminium oxide and the titanium dioxide of high-purity are mixed into additive and are prepared, wherein magnesia Content >=85wt%, relative density >=95%, additive level 15wt%.The technique includes the following steps:
A. nano magnesia, zirconium oxide, yttrium oxide, aluminium oxide and titanium dioxide raw material powder are formed according to a certain percentage It weighs, is uniformly mixed；
B. the step a powder being uniformly mixed and water are put into progress low temperature liquid phase ball milling, ball-milling medium in ball grinder or sand mill For the zirconia ceramics ball that high purity yttria is stable, wet-milling mixing 2-40 hours, the ceramic slurry being uniformly mixed；
C. ceramic slurry made from step b is spray-dried, the diameter of particle after control is dry, obtain good fluidity, Particle size is 2-100 μm, the ceramic powder of bulk density 0.5-3.0g/cm3, i.e. completion granulation process；
D. the ceramic powder after being granulated made from step c is subjected to high-pressure molding and obtains ceramic body, the pressure generallyd use exists It forms within pressure maintaining 2-30 minutes under 10-300MPa pressure, i.e. completion preprocessing processing；
E. ceramic body made from step d is obtained in high temperature sintering furnace according to default sintering schedule high temperature sintering and is based on receiving The magnesium oxide-based magnesia ceramics of rice.
The nano magnesia, zirconium oxide, yttrium oxide, aluminium oxide and titanium dioxide raw material powder mass ratio be 85:0 ~ 8:0 ~ 2:0 ~ 7:0 ~ 4.
The mass ratio of the mixed powder and water is 30-70:100, and the low temperature liquid phase ball milling temperature is 0-10 DEG C, The ball-milling medium size is 0.8mm or 0.4mm.
The temperature of the spray drying is 180-300 DEG C.
The default sintering schedule be with the heating rate of 1 DEG C/min-20 DEG C/min from room temperature to 300-400 DEG C heat preservation 20-100 minute, 800 DEG C -1000 DEG C are warming up to the heating rate of 1 DEG C/min-15 DEG C/min, heat preservation 20- 100 minutes, 1400-1600 DEG C of heat preservation 1-10 hours is warming up to the heating rate of 1 DEG C/min-10 DEG C/min, with 1 DEG C The heating rate of/min-5 DEG C/min is warming up to 1700-1800 DEG C of heat preservation 1-10 hours, then with 1 DEG C/min-20 DEG C/ The rate of temperature fall of min is cooled to room temperature.
Beneficial effects of the present invention:
Nano oxidized magnesium-based ceramics produced by the present invention have the characteristics that consistency height, purity is high, high temperature resistant, corrosion-resistant, can grow Phase is applied to the environment such as high temperature, the highly corrosive such as high-temperature calcination, metal smelt, stable preparation process of the present invention, high yield rate, suitable It answers range wide, is suitable for mass production, and do not limited by specific ceramic shape, suitable for preparing the oxidation of various sizes, shape Magnesium ceramics, ceramic body sintering rejection rate after molding are almost nil.
Detailed description of the invention
The SEM of Fig. 1 case study on implementation sample 1 schemes.
Specific embodiment
The present invention is described in detail below by specific example, but protection scope of the present invention is not only restricted to these Examples of implementation.
Embodiment 1: by nano magnesia, zirconium oxide, yttrium oxide, alumina raw material powder according to 85:8:2:5 ratio group At weighing, it is uniformly mixed；Uniformly mixed powder and water are put into sand mill by the mass ratio of 30:100 and carry out low temperature liquid phase Ball milling, at 0 DEG C, ball-milling medium is the stable zirconia ceramics ball of 0.8mm high purity yttria for temperature control, and wet-milling mixing 2 is small When, the ceramic slurry that is uniformly mixed；Ceramic slurry is spray-dried, temperature is 180 DEG C, the powder after control is dry Partial size, obtaining good fluidity, particle size is 2-10 μm, the ceramic powder of bulk density 3.0g/cm3, that is, completes to be granulated Journey；Ceramic powder after granulation is subjected to high-pressure molding and obtains ceramic body, the pressure generallyd use is protected under 10MPa pressure It presses 30 minutes and forms, is i.e. completion preprocessing processing；By ceramic body obtained according to default sintering schedule in high temperature sintering furnace High temperature sintering obtains the magnesia ceramics based on nano oxidized magnesium-based, and presetting sintering schedule is with the heating rate of 20 DEG C/min 20 minutes are kept the temperature from room temperature to 300 DEG C, 800 DEG C is warming up to the heating rate of 15 DEG C/min, keeps the temperature 20 minutes, with The heating rate of 10 DEG C/min is warming up to 1400 DEG C and keeps the temperature 1 hour, is warming up to 1700 DEG C with the heating rate of 5 DEG C/min Heat preservation 10 hours, is then cooled to room temperature with the rate of temperature fall of 20 DEG C/min.
Embodiment 2: by nano magnesia, zirconium oxide, yttrium oxide, aluminium oxide and titanium dioxide raw material powder according to 85: The ratio of 4:2:7:2, which forms, to be weighed, and is uniformly mixed；Uniformly mixed powder and water are put into ball grinder by the mass ratio of 50:100 Middle progress low temperature liquid phase ball milling, at 10 DEG C, ball-milling medium is the stable zirconia ceramics of 0.4mm high purity yttria for temperature control Ball, wet-milling mixing 5 hours, the ceramic slurry being uniformly mixed；Ceramic slurry is spray-dried, temperature is 300 DEG C, control Diameter of particle after system is dry obtains good fluidity, particle size is 50-100 μm, the ceramic powder of bulk density 1.5g/cm3 Body, i.e. completion granulation process；Ceramic powder after granulation is subjected to high-pressure molding and obtains ceramic body, the pressure generallyd use exists It forms within pressure maintaining 5 minutes under 300MPa pressure, i.e. completion preprocessing processing；Ceramic body obtained is pressed in high temperature sintering furnace According to default sintering schedule high temperature sintering obtain the magnesia ceramics based on nano oxidized magnesium-based, preset sintering schedule be with 20 DEG C/ The heating rate of min keeps the temperature 50 minutes from room temperature to 400 DEG C, is warming up to 900 DEG C with the heating rate of 15 DEG C/min, Heat preservation 50 minutes is warming up to 1500 DEG C with the heating rate of 10 DEG C/min and keeps the temperature 5 hours, with the heating rate of 2 DEG C/min It is warming up to 1800 DEG C and keeps the temperature 4 hours, be then cooled to room temperature with the rate of temperature fall of 10 DEG C/min.
Embodiment 3: by nano magnesia, zirconium oxide, yttrium oxide, aluminium oxide and titanium dioxide raw material powder according to 85: The ratio of 5:1:5:4, which forms, to be weighed, and is uniformly mixed；Uniformly mixed powder and water are put into ball grinder by the mass ratio of 70:100 Middle progress low temperature liquid phase ball milling, at 5 DEG C, ball-milling medium is the stable zirconia ceramics of 0.4mm high purity yttria for temperature control Ball, wet-milling mixing 10 hours, the ceramic slurry being uniformly mixed；Ceramic slurry is spray-dried, temperature is 230 DEG C, Diameter of particle after control is dry obtains good fluidity, particle size is 20-50 μm, the ceramic powder of bulk density 2.5g/cm3 Body, i.e. completion granulation process；Ceramic powder after granulation is subjected to high-pressure molding and obtains ceramic body, the pressure generallyd use exists It forms within pressure maintaining 2 minutes under 50MPa pressure, i.e. completion preprocessing processing；Ceramic body obtained is pressed in high temperature sintering furnace According to default sintering schedule high temperature sintering obtain the magnesia ceramics based on nano oxidized magnesium-based, preset sintering schedule be with 1 DEG C/ The heating rate of min keeps the temperature 100 minutes from room temperature to 400 DEG C, is warming up to 1000 with the heating rate of 1 DEG C/min DEG C, 100 minutes are kept the temperature, 1600 DEG C is warming up to the heating rate of 1 DEG C/min and keeps the temperature 10 hours, with the heating of 1 DEG C/min Rate is warming up to 1800 DEG C and keeps the temperature 1 hour, is then cooled to room temperature with the rate of temperature fall of 1 DEG C/min.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (6)

1. a kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness, which is characterized in that use high-purity nano magnesia For raw material, zirconium oxide, yttrium oxide, aluminium oxide and the titanium dioxide of high-purity are mixed into additive and are prepared, wherein aoxidizing Content of magnesium >=85wt%, relative density >=95%, additive level 15wt%.
2. the technique includes the following steps:
A. nano magnesia, zirconium oxide, yttrium oxide, aluminium oxide and titanium dioxide raw material powder are formed according to a certain percentage It weighs, is uniformly mixed；
B. the step a powder being uniformly mixed and water are put into progress low temperature liquid phase ball milling, ball-milling medium in ball grinder or sand mill For the zirconia ceramics ball that high purity yttria is stable, wet-milling mixing 2-40 hours, the ceramic slurry being uniformly mixed；
C. ceramic slurry made from step b is spray-dried, the diameter of particle after control is dry, obtain good fluidity, Particle size is 2-100 μm, the ceramic powder of bulk density 0.5-3.0g/cm3, i.e. completion granulation process；
D. the ceramic powder after being granulated made from step c is subjected to high-pressure molding and obtains ceramic body, the pressure generallyd use exists It forms within pressure maintaining 2-30 minutes under 10-300MPa pressure, i.e. completion preprocessing processing；
E. ceramic body made from step d is obtained in high temperature sintering furnace according to default sintering schedule high temperature sintering and is based on receiving The magnesium oxide-based magnesia ceramics of rice.
3. a kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness according to claim 1, which is characterized in that step Nano magnesia described in rapid a, zirconium oxide, yttrium oxide, aluminium oxide and titanium dioxide raw material powder mass ratio be 85:0 ~ 8:0 ~ 2:0 ~ 7:0 ~ 4.
4. a kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness according to claim 1, which is characterized in that step The mass ratio of mixed powder described in rapid b and water is 30-70:100, and the low temperature liquid phase ball milling temperature is 0-10 DEG C, institute The ball-milling medium size stated is 0.8mm or 0.4mm.
5. a kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness according to claim 1, which is characterized in that step The temperature of spray drying described in rapid c is 180-300 DEG C.
6. a kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness according to claim 1, which is characterized in that step In rapid e, the default sintering schedule be with the heating rate of 1 DEG C/min-20 DEG C/min from room temperature to 300-400 DEG C Heat preservation 20-100 minutes is warming up to 800 DEG C -1000 DEG C with the heating rate of 1 DEG C/min-15 DEG C/min, keeps the temperature 20-100 Minute, 1400-1600 DEG C of heat preservation 1-10 hours is warming up to the heating rate of 1 DEG C/min-10 DEG C/min, with 1 DEG C/ The heating rate of min-5 DEG C/min is warming up to 1700-1800 DEG C of heat preservation 1-10 hours, then with 1 DEG C/min-20 DEG C/ The rate of temperature fall of min is cooled to room temperature.
CN201810901429.6A 2018-08-09 2018-08-09 A kind of preparation method of the nano oxidized magnesium-based ceramics of high-compactness Pending CN108947493A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109437858A (en) * 2018-12-29 2019-03-08 南京宝淳新材料科技有限公司 A kind of magnesia ceramics powder and preparation method thereof
CN110256065A (en) * 2019-07-19 2019-09-20 陕西科技大学 A kind of dense oxide titanium nano ceramics and its preparation method and application
CN111848133A (en) * 2020-06-09 2020-10-30 西昌学院 Preparation method of high-thermal-shock-resistance magnesium oxide ceramic

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103601473A (en) * 2013-11-04 2014-02-26 中国科学院合肥物质科学研究院 High-purity high-density magnesium-oxide ceramic and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103601473A (en) * 2013-11-04 2014-02-26 中国科学院合肥物质科学研究院 High-purity high-density magnesium-oxide ceramic and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘锦方: "《结构材料学》", 29 February 2008, 哈尔滨工业大学出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109437858A (en) * 2018-12-29 2019-03-08 南京宝淳新材料科技有限公司 A kind of magnesia ceramics powder and preparation method thereof
CN110256065A (en) * 2019-07-19 2019-09-20 陕西科技大学 A kind of dense oxide titanium nano ceramics and its preparation method and application
CN111848133A (en) * 2020-06-09 2020-10-30 西昌学院 Preparation method of high-thermal-shock-resistance magnesium oxide ceramic

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Application publication date: 20181207