CN101508561A - Process for producing LaPO4/ZTA composite ceramic with evenly distributed LaPO4 - Google Patents

Process for producing LaPO4/ZTA composite ceramic with evenly distributed LaPO4 Download PDF

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Publication number
CN101508561A
CN101508561A CNA2009100199688A CN200910019968A CN101508561A CN 101508561 A CN101508561 A CN 101508561A CN A2009100199688 A CNA2009100199688 A CN A2009100199688A CN 200910019968 A CN200910019968 A CN 200910019968A CN 101508561 A CN101508561 A CN 101508561A
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China
Prior art keywords
lapo
suspension
lapo4
preparation
zta
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Pending
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CNA2009100199688A
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Chinese (zh)
Inventor
王昕�
郑秋菊
宫承鹏
尹衍升
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Ocean University of China
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Ocean University of China
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Priority to CNA2009100199688A priority Critical patent/CN101508561A/en
Publication of CN101508561A publication Critical patent/CN101508561A/en
Pending legal-status Critical Current

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Abstract

A method for preparing LaPO4/ZTA composite ceramics on which LaPO4 is evenly dispersed and distributed is characterized in that firstly, compound powders of alpha-Al2O3 and ZrO2 are put into deionized water and dispersant is added for ultrasonic dispersion to prepare suspension; secondly, La(NO3)3 aqueous solution is added into the suspension and stirred magnetically, and then Na3PO4 aqueous solution with volume and concentration equal to the volume and concentration of the La(NO3)3 aqueous solution is dropped into the suspension under magnetic stirring, with 5-15 drops per minute; during dropping, the pH value of the suspension keeps constant; after dropping, the suspension is stirred continuously for 1-3h, then foreign ions in the suspension are removed, and the suspension is dried in a drying oven, thus obtaining LaPO4 coated compound powders of the alpha-Al2O3 and ZrO2; finally, the coated powders are subjected to hot pressed sintering. The method takes the lead to introduce the coating method to the preparation of the LaPO4/ZTA composite and is simple in steps and easy in control, which not only can obtain the weak interfaces between LaPO4 and Al2O3 as well as ZrO2 but also can reduce the content of the soft phase LaPO4. Such a design can achieve good processability by sacrificing less mechanical property.

Description

A kind of LaPO 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics
Technical field
The present invention relates to a kind of preparation method of inorganic materials, particularly relate to a kind of LaPO 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics.
Background technology
ZTA (ZrO 2Toughness reinforcing Al 2O 3) composite ceramics possesses good corrosion resistance, thermal shock resistance, higher intensity and toughness, might solve reliability and endurance issues that the restriction ceramic material is used, have broad application prospects.But the workability of ZTA composite ceramics is still being limited to it to a great extent in many-sided popularization.In order to improve the machinability of ZTA ceramic material, people are LaPO 4Join Al 2O 3, ZrO 2In the matrix, broken through the restriction of pottery on processing characteristics, made ceramic material have more wide application prospect.RE phosphate/oxide compound composite ceramics is a kind of novel processable ceramic by U.S. Rockwell scientific center research report in 1998, key between phosphoric acid salt and the oxide compound is a weak bond, add and on the interface, form being connected of tiny crack and tiny crack in man-hour, thereby make this composite diphase material become high performance processable ceramics material.This composite ceramics has good chemical compatibility, and its fusing point height has excellent stability under oxidizing atmosphere.LaPO 4Soft mutually the effect be the machinable important mechanism of material; Generally along with LaPO 4The increase of addition, the machinability of material improves, and what still bring but is the significantly decline of mechanical property, and general traditional method is with LaPO 4And Al 2O 3, ZrO 2Directly mix, need LaPO 4Amount more, and LaPO 4Be again weak phase, add the mechanical properties decrease that can make too much material, how alleviating this contradiction is the emphasis place of processable ceramic research.At present, prepare LaPO with method for coating 4The LaPO that even dispersion distributes 4/ ZTA composite ceramics does not also have relevant report both at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of LaPO 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is to overcome above shortcomings in the prior art.
A kind of LaPO 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that selecting La (NO 3) 36H 2O, NaPO 412H 2O and α-Al 2O 3, ZrO 2As raw material, with La (NO 3) 36H 2O and Na 3PO 412H 2O is made into respectively the certain density aqueous solution; With a certain proportion of Al 2O 3, ZrO 2Composite granule is put into deionized water, adds dispersant ammonium polymethacrylate (PMAA), and suspension is made in ultrasonic dispersion; Then with La (NO 3) 3The aqueous solution joins in this suspension, with agitator magnetic agitation 30~100min; Then with the isocyatic above-mentioned Na of equal-volume 3PO 4The aqueous solution splashes into this suspension, and the control rate of addition is 5~15/min, in the dropping process, makes the pH value of suspension keep constant; After dripping end, suspension is continued to stir 1~3h again, with deionized water foreign ion is wherein cleaned then, put into the drying box drying, obtain LaPO 4Coating alpha-Al 2O 3, ZrO 2Composite granule; At last coated powder is carried out hot pressed sintering.
The present invention takes the lead in method for coating is introduced into LaPO 4In/ZTA the composite manufacture, step is simple, easy to control, both can obtain LaPO 4And Al 2O 3, ZrO 2Between weak interface, can reduce soft phase LaPO again 4Content, by such design, can sacrifice littler mechanical property and obtain preferably processing characteristics, overcome LaPO 4The difficult problem of/ZTA pottery aspect processing makes it obtain further promotion and application.
Description of drawings
Accompanying drawing is the LaPO of the present invention with the method for coating preparation 4The LaPO that even dispersion distributes 4The fracture SEM picture of/ZTA composite ceramics.
Embodiment
The present invention selects La (NO 3) 36H 2O, NaPO 412H 2O and α-Al 2O 3, ZrO 2As raw material, Al in the composite granule 2O 3With ZrO 2Mass ratio be 4:1, volume ratio is 6.26:1.With La (NO 3) 36H 2O and Na 3PO 412H 2O is made into respectively the aqueous solution of 0.01mol/L.With an amount of α-Al 2O 3, ZrO 2Composite powder is put into deionized water, adds dispersant ammonium polymethacrylate (PMAA), and suspension is made in ultrasonic dispersion.Then with La (NO 3) 3The aqueous solution joins in this suspension, uses the agitator magnetic agitation.Then with the isocyatic above-mentioned Na of equal-volume 3PO 4The aqueous solution splashes into this suspension, and the control rate of addition is at 15/min, and in the dropping process, making the pH value of suspension constant is 10.After dropping finishes, suspension is continued to stir 2h again, then with deionized water that foreign ion wherein is clean, put into 60 ℃ of lower dry 12h of drying box, obtain LaPO 4Coating alpha-Al 2O 3, ZrO 2Composite granule.Make LaPO in this way 4Content is 20% coated powder, then with it at 1500 ℃ of hot pressed sintering 2h, just obtain LaPO 4The LaPO that even dispersion distributes 4/ ZTA composite ceramics.
Accompanying drawing is the LaPO of the present invention with the method for coating preparation 4The LaPO that even dispersion distributes 4The fracture back scattering SEM picture of/ZTA composite ceramics, its LaPO 4Content be 20%.White particle is LaPO among the figure 4, grizzled particle is Al 2O 3And ZrO 2(because La and Al, Zr atomic number differ bigger, LaPO in the picture 4Differ bigger with other two kinds of phase contrasts, more easily differentiate).LaPO among the figure 4With the formal distribution of membranaceous or nano-scale particle at Al 2O 3And ZrO 2Around the particle.The processability of processable ceramics material is mainly derived from soft and the weak interface of matrix and the cleavage of soft phase self, LaPO 4With the formal distribution of membranaceous or nano-scale particle at Al 2O 3Around the particle, realized LaPO 4At LaPO 4Even dispersion in the/ZTA composite ceramics distributes, and has increased the area of weak interface, and nano level LaPO 4Particle can play crack deflection in the process of Materials Fracture, the effect that consumed energy etc. are toughness reinforcing, thus realized reducing soft phase LaPO 4Content, improve the purpose of the machinability of material.
α-Al described in the present invention 2O 3, ZrO 2The average grain diameter of particle is 50~300nm; Described La (NO 3) 36H 2O and NaPO 412H 2The concentration of the O aqueous solution is 0.001~0.1mol/L; Al in the described composite granule 2O 3With ZrO 2Mass ratio be 2~6:1, Al 2O 3, ZrO 2The weight ratio scope of composite granule and deionized water is 1:50~300, and the concentration of dispersant ammonium polymethacrylate in suspension of adding is 0.1~1wt%; The pH value scope of suspension is 1~12 in the described dropping process; Described baking temperature is 40~100 ℃, and be 8~16h drying time; Described dispersant is ammonium polymethacrylate, polyethylene glycol or citric acid; Described LaPO 4Content is 10%~40%; The temperature of described hot pressed sintering is 1400 ℃~1600 ℃, and the time is 1h~3h.

Claims (9)

1, a kind of LaPO 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that selecting La (NO 3) 36H 2O, NaPO 412H 2O and α-Al 2O 3, ZrO 2As raw material, with La (NO 3) 36H 2O and Na 3PO 412H 2O is made into respectively the certain density aqueous solution; With a certain proportion of Al 2O 3, ZrO 2Composite granule is put into deionized water, adds dispersant ammonium polymethacrylate (PMAA), and suspension is made in ultrasonic dispersion; Then with La (NO 3) 3The aqueous solution joins in this suspension, with agitator magnetic agitation 30~100min; Then with the isocyatic above-mentioned Na of equal-volume 3PO 4The aqueous solution splashes into this suspension, and the control rate of addition is 5~15/min, in the dropping process, makes the pH value of suspension keep constant; After dripping end, suspension is continued to stir 1~3h again, with deionized water foreign ion is wherein cleaned then, put into the drying box drying, obtain LaPO 4Coating alpha-Al 2O 3, ZrO 2Composite granule; At last coated powder is carried out hot pressed sintering.
2, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that described α-Al 2O 3, ZrO 2The average grain diameter of composite granule is about 50~300nm.
3, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that described La (NO 3) 36H 2O and NaPO 412H 2The concentration of the O aqueous solution is 0.001~0.1mol/L.
4, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that described Al 2O 3, ZrO 2Al in the composite granule 2O 3With ZrO 2Mass ratio be 2~6:1, Al 2O 3, ZrO 2The weight ratio scope of composite granule and deionized water is 1:50~300, and the concentration of dispersant ammonium polymethacrylate in suspension of adding is 0.1~1wt%.
5, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that the pH value scope of suspension in the described dropping process is 1~12.
6, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that described drying temperature is 40~100 ℃, and be 8~16h time of drying.
7, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that described dispersion agent is ammonium polymethacrylate, polyoxyethylene glycol or citric acid.
8, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics is characterized in that described LaPO 4Content is 10%~40%.
9, LaPO as claimed in claim 1 4The LaPO that even dispersion distributes 4The preparation method of/ZTA composite ceramics, the temperature that it is characterized in that described hot pressed sintering are 1400 ℃~1600 ℃, and the time is 1h~3h.
CNA2009100199688A 2009-03-21 2009-03-21 Process for producing LaPO4/ZTA composite ceramic with evenly distributed LaPO4 Pending CN101508561A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2674135C2 (en) * 2013-02-25 2018-12-04 Люмиледс Холдинг Б.В. Coated luminescent particle, luminescent converter element, light source, luminaire and method of manufacturing a coated luminescent particle
CN115043665A (en) * 2022-06-07 2022-09-13 哈尔滨工业大学 Porous mullite-lanthanum phosphate complex phase wave-transmitting material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101269975A (en) * 2008-04-29 2008-09-24 中国海洋大学 Heterogeneous nucleation preparation method for LaPO4 coating alpha-Al2O3 powder body

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101269975A (en) * 2008-04-29 2008-09-24 中国海洋大学 Heterogeneous nucleation preparation method for LaPO4 coating alpha-Al2O3 powder body

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2674135C2 (en) * 2013-02-25 2018-12-04 Люмиледс Холдинг Б.В. Coated luminescent particle, luminescent converter element, light source, luminaire and method of manufacturing a coated luminescent particle
US10875005B2 (en) 2013-02-25 2020-12-29 Lumileds Llc Coated luminescent particle, a luminescent converter element, a light source, a luminaire and a method of manufacturing a coated luminescent particle
CN115043665A (en) * 2022-06-07 2022-09-13 哈尔滨工业大学 Porous mullite-lanthanum phosphate complex phase wave-transmitting material and preparation method thereof

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Application publication date: 20090819