CN102775149A - Preparation method for praseodymium oxide-added silicon nitride composite ceramic - Google Patents
Preparation method for praseodymium oxide-added silicon nitride composite ceramic Download PDFInfo
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- CN102775149A CN102775149A CN201110118695XA CN201110118695A CN102775149A CN 102775149 A CN102775149 A CN 102775149A CN 201110118695X A CN201110118695X A CN 201110118695XA CN 201110118695 A CN201110118695 A CN 201110118695A CN 102775149 A CN102775149 A CN 102775149A
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Abstract
The invention relates to the technical field of ceramic materials and specifically to a method for preparing a high performance silicon nitride (Si3N4) ceramic through pressureless sintering by using praseodymium oxide as an additive. The ceramic comprises the following components expressed in mass percent: 6 to 12% of praseodymium oxide and 88 to 94% of silicon nitride. The objective of the invention is to provide the method for preparing the high performance silicon nitride ceramic through pressureless sintering by using praseodymium oxide as the additive to overcome disadvantages in the prior art, and the prepared ceramic can be extensively used for preparation of components and parts used in fields like the chemistry industry, machinery, metallurgy and the aerospace industry.
Description
[technical field]
The present invention relates to a kind of technical field of ceramic material, specifically is a kind of Praseodymium trioxide (Pr
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 Praseodymium 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 Praseodymium 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 Praseodymium 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 Praseodymium trioxide involved in the present invention is produced as additive pressureless sintering, component and mass percentage content are: Praseodymium trioxide 7%～12%, silicon nitride 88%～93%.
5～7 microns of described Praseodymium trioxide granularities, 0.4～0.7 micron of silicon nitride granularity.
The silicon nitride ceramics method that Praseodymium trioxide involved in the present invention is produced as additive pressureless sintering comprises the steps:
Step 1 takes by weighing Praseodymium 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, Praseodymium 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 Praseodymium trioxide is 7%～12%, and the weight percent of silicon nitride is 88%～93%.
In the step 1, α-Si in the said silicon nitride
3N
4Content is greater than 90%.
In the step 1, Pr in the said Praseodymium 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 Praseodymium 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
Praseodymium trioxide is Ganzhou Jiarun novel material ltd, and silicon nitride powder is the M11 powder that German Starck company produces.Take by weighing 9% Praseodymium trioxide and 91% 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 3.32g/cm
3, folding strength is 683Mpa.
Claims (7)
1. silicon nitride adds the silicon nitride ceramics that the related Praseodymium trioxide of composite ceramics preparation method of Praseodymium trioxide is produced as additive pressureless sintering, and component and mass percentage content are: Praseodymium trioxide 7%～12%, silicon nitride 88%～93%.5～7 microns of described Praseodymium trioxide granularities, 0.4～0.7 micron of silicon nitride granularity.
2. the silicon nitride ceramics method that the related Praseodymium trioxide of composite ceramics preparation method of silicon nitride interpolation Praseodymium trioxide according to claim 1 is produced as additive pressureless sintering comprises the steps:
Step 1 takes by weighing Praseodymium 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, Praseodymium 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. silicon nitride according to claim 2 adds the composite ceramics preparation method of Praseodymium trioxide, and the weight percent that it is characterized in that Praseodymium trioxide described in the step 1 is 7%～12%, and the weight percent of silicon nitride is 88%～93%.
4. silicon nitride according to claim 2 adds the composite ceramics preparation method of Praseodymium trioxide, it is characterized in that in the step 1 α-Si in the said silicon nitride
3N
4Content is greater than 90%.
5. silicon nitride according to claim 2 adds the composite ceramics preparation method of Praseodymium trioxide, it is characterized in that in the step 1 Pr in the said Praseodymium trioxide
2O
3Content is greater than 98%.
6. silicon nitride according to claim 2 adds the composite ceramics preparation method of Praseodymium trioxide, it is characterized in that in the step 3 that said nitrogen gas pressure is 1～2 normal atmosphere.
7. silicon nitride according to claim 2 adds the composite ceramics preparation method of Praseodymium trioxide, it is characterized in that in the step 4 that said mechanical property is a folding strength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110118695XA CN102775149A (en) | 2011-05-10 | 2011-05-10 | Preparation method for praseodymium oxide-added silicon nitride composite ceramic |
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|---|---|---|---|
| CN201110118695XA CN102775149A (en) | 2011-05-10 | 2011-05-10 | Preparation method for praseodymium oxide-added silicon nitride composite ceramic |
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| CN102775149A true CN102775149A (en) | 2012-11-14 |
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| CN201110118695XA Pending CN102775149A (en) | 2011-05-10 | 2011-05-10 | Preparation method for praseodymium oxide-added silicon nitride composite ceramic |
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2011
- 2011-05-10 CN CN201110118695XA patent/CN102775149A/en active Pending
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Addressee: Kunshan Zhiji Material Technology Co., Ltd. Document name: Notification that Application Deemed to be Withdrawn |
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Application publication date: 20121114 |