CN102557648A - Preparation method of silicon nitride-doped holimium oxide ceramic - Google Patents
Preparation method of silicon nitride-doped holimium oxide ceramic Download PDFInfo
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- CN102557648A CN102557648A CN2010105881197A CN201010588119A CN102557648A CN 102557648 A CN102557648 A CN 102557648A CN 2010105881197 A CN2010105881197 A CN 2010105881197A CN 201010588119 A CN201010588119 A CN 201010588119A CN 102557648 A CN102557648 A CN 102557648A
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- silicon nitride
- holmium trioxide
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- trioxide
- holmium
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Abstract
The invention relates to the technical field of a ceramic material, in particular to a method for producing high-performance silicon nitride (Si3N4) by adopting holimium oxide (Ho2O3) as an additive via pressureless sintering. The component and mass percentages are as follows: 3-12% of holimium oxide and 85-97% of silicon nitride. The invention aims at overcoming disadvantages of the prior art and providing a method for producing high-performance silicon nitride by adopting holimium oxide as the additive via pressureless sintering. The method can be widely applied to preparing parts in fields such as chemical industry, machinery, metallurgy, aerospace and the like.
Description
[technical field]
The present invention relates to a kind of technical field of ceramic material, specifically is a kind of Holmium trioxide (Ho
2O
3) as additive pressureless sintering production high-performance silicon nitride (Si
3N
4) ceramic method.
[background technology]
Silicon nitride ceramics has excellent mechanical behavior under high temperature, is acknowledged as one of the most rising high temperature resistant structure ceramics.Silicon nitride is as a kind of covalent linkage platform thing, and spread coefficient is little, does not have fusing point, decomposes ammonification and silicon about 2173K, is difficult to sintering.Common silicon nitride ceramics respond sintering and hot pressed sintering, the reaction sintering density is poor, poor mechanical property, though hot pressed sintering density is high, mechanical property is good, cost is higher, is difficult to scale operation.And pressureless sintering falls between, because silicon nitride ceramics is the covalent linkage compound, and the pressureless sintering difficulty, the density that improves the pressureless sintering silicon nitride ceramics becomes the research focus, adds rare earth oxide usually as sintering aid, like iridium oxide.But the cost of iridium oxide is higher, and is unfavorable for the application of silicon nitride.We select for use Holmium trioxide as sintered density and the mechanical property of additive to improve silicon nitride for this reason.
[summary of the invention]
The objective of the invention is to overcome the deficiency of prior art, the method for a kind of Holmium trioxide as additive pressureless sintering production high-performance silicon nitride ceramics is provided.Working method of the present invention is simple, and cost is low, is prone to realize industrialization production; The silicon nitride ceramics that Holmium trioxide of the present invention is produced as additive pressureless sintering has the density height, the characteristics that mechanical property is good.
The present invention realizes through following technical scheme:
The silicon nitride ceramics that Holmium trioxide involved in the present invention is produced as additive pressureless sintering, component and mass percentage content are: Holmium trioxide 3%~12%, silicon nitride 85%~97%.
3~7 microns of described Holmium trioxide granularities, 0.4~0.8 micron of silicon nitride granularity.
The silicon nitride ceramics method that Holmium trioxide involved in the present invention is produced as additive pressureless sintering comprises the steps:
Step 1 takes by weighing Holmium trioxide and silicon nitride ceramics powder respectively, in planetary ball mill, changes mixing 2 hours with PM 270~330; Dispersion medium is an absolute ethyl alcohol; 60 ℃ of oven dry, the time is 2~3 hours subsequently, Holmium trioxide that obtains mixing and silicon nitride ceramics mixed powder;
Step 2 at 75~100Mpa forming under the pressure, forms biscuit with the mixed powder of step 1;
Step 3, with the biscuit in the step 2 in vacuum carbon tube furnace under nitrogen protection, under 1400~1550 ℃ of temperature, be incubated 12~18 hours.
Step 4 is taken out the silicon nitride ceramics that burns till in the step 3 detection volume density and mechanical property.
In the step 1, the weight percent of said Holmium trioxide is 3%~12%, and the weight percent of silicon nitride is 85%~97%.
In the step 1, α-Si in the said silicon nitride
3N
4Content is greater than 90%.
In the step 1, Ho in the said Holmium trioxide
2O
3Content is greater than 98%.
In the step 3, said nitrogen gas pressure is 1~2 normal atmosphere.
In the step 4, said mechanical property is a folding strength.
Among the present invention, described Holmium trioxide plays the effect of sintering aid, under 1400~1550 ℃ of high temperature sintering conditions, forms liquid phase, makes the silicon nitride ceramics densification.
The present invention has following beneficial effect: the silicon nitride ceramics compactness extent is high, and mechanical property is good, satisfies the actual needs that use.This preparation method is simple, and cost is low, is prone to realize industrialization production.
[embodiment]
Below in conjunction with embodiment the present invention is described further.Production technology of the present invention is to implement easily to this professional people.Present embodiment provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
The Holmium trioxide powder is own synthesis material, and silicon nitride powder is the M11 powder that German Starck company produces.Take by weighing 7% Holmium trioxide powder and 93% silicon nitride powder respectively according to weight percent.
Above-mentioned two kinds of powder (QM-3SP2 of Nanjing Univ. Instrument Factory type) in planetary ball mill are mixed, and rotating speed 300 changes 1.5 hours time.With the forming under the pressure of powder mix, biscuit (the flourish electric furnace ZT-40-20 of ltd of Shanghai occasion type) 1450 ℃ in vacuum carbon tube furnace is incubated 16 hours at 80Mpa.
The volume density of the silicon nitride ceramics that present embodiment obtains is 3.29g/cm
3, folding strength is 673Mpa.
Claims (7)
1. the silicon nitride ceramics produced as additive pressureless sintering of the related Holmium trioxide of the preparation method of silicon nitride doping Holmium trioxide pottery, component and mass percentage content are: Holmium trioxide 3%~12%, silicon nitride 85%~97%.3~7 microns of described Holmium trioxide granularities, 0.4~0.8 micron of silicon nitride granularity.
2. the silicon nitride ceramics method that the related Holmium trioxide of the preparation method of silicon nitride doping Holmium trioxide pottery according to claim 1 is produced as additive pressureless sintering comprises the steps:
Step 1 takes by weighing Holmium trioxide and silicon nitride ceramics powder respectively, in planetary ball mill, changes mixing 2 hours with PM 270~330; Dispersion medium is an absolute ethyl alcohol; 60 ℃ of oven dry, the time is 2~3 hours subsequently, Holmium trioxide that obtains mixing and silicon nitride ceramics mixed powder;
Step 2 at 75~100Mpa forming under the pressure, forms biscuit with the mixed powder of step 1;
Step 3, with the biscuit in the step 2 in vacuum carbon tube furnace under nitrogen protection, under 1400~1550 ℃ of temperature, be incubated 12~18 hours.
Step 4 is taken out the silicon nitride ceramics that burns till in the step 3 detection volume density and mechanical property.
3. the preparation method of silicon nitride doping Holmium trioxide pottery according to claim 2, the weight percent that it is characterized in that said Holmium trioxide is 3%~12%, the weight percent of silicon nitride is 85%~97%.
4. the preparation method of silicon nitride doping Holmium trioxide pottery according to claim 2 is characterized in that in the step 1 α-Si in the said silicon nitride
3N
4Content is greater than 90%.
5. the preparation method of silicon nitride doping Holmium trioxide pottery according to claim 2 is characterized in that in the step 1 Ho in the said Holmium trioxide
2O
3Content is greater than 98%.
6. the preparation method of silicon nitride doping Holmium trioxide pottery according to claim 2 is characterized in that in the step 3 that said nitrogen gas pressure is 1~2 normal atmosphere.
7. the preparation method of silicon nitride doping Holmium trioxide pottery according to claim 2 is characterized in that in the step 4 that said mechanical property is a folding strength.
Priority Applications (1)
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CN2010105881197A CN102557648A (en) | 2010-12-14 | 2010-12-14 | Preparation method of silicon nitride-doped holimium oxide ceramic |
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CN2010105881197A CN102557648A (en) | 2010-12-14 | 2010-12-14 | Preparation method of silicon nitride-doped holimium oxide ceramic |
Publications (1)
Publication Number | Publication Date |
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CN102557648A true CN102557648A (en) | 2012-07-11 |
Family
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CN2010105881197A Pending CN102557648A (en) | 2010-12-14 | 2010-12-14 | Preparation method of silicon nitride-doped holimium oxide ceramic |
Country Status (1)
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2010
- 2010-12-14 CN CN2010105881197A patent/CN102557648A/en active Pending
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Addressee: Lu Shuping Document name: Notification that Application Deemed to be Withdrawn |
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WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120711 |