CN102531615A - Process for producing silicon nitride ceramic stabilized by rare-earth praseodymium and holmium - Google Patents
Process for producing silicon nitride ceramic stabilized by rare-earth praseodymium and holmium Download PDFInfo
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- CN102531615A CN102531615A CN2010106009711A CN201010600971A CN102531615A CN 102531615 A CN102531615 A CN 102531615A CN 2010106009711 A CN2010106009711 A CN 2010106009711A CN 201010600971 A CN201010600971 A CN 201010600971A CN 102531615 A CN102531615 A CN 102531615A
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Abstract
The invention relates to the technical field of ceramic materials, in particular to a method for producing high-performance silicon nitride (Si3N4) ceramic through pressureless sintering by taking praseodymium oxide and holmium oxide as additives. The ceramic comprises the following components in percentage by mass: 3 to 7 percent of holmium oxide, 5 to 8 percent of praseodymium oxide and 85 to 92 percent of Si3N4. The method for producing the high-performance Si3N4 ceramic through pressureless sintering by taking the praseodymium oxide and the holmium oxide as the additives aims to overcome the shortcomings in the prior art, and can be widely applied to manufacturing of parts used 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 the method for a kind of Holmium trioxide Praseodymium trioxide as additive pressureless sintering production high-performance silicon nitride ceramics.
[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 the Holmium trioxide 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 Holmium trioxide 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 Holmium trioxide 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 Holmium trioxide Praseodymium trioxide involved in the present invention is produced as additive pressureless sintering, component and mass percentage content are: Holmium trioxide 3%～7%, Praseodymium trioxide 5%～8%, silicon nitride 85%～92%.
3～6 microns of described Holmium trioxide granularities, 5～7 microns of Praseodymium trioxide granularities, 0.4～0.7 micron of silicon nitride granularity.
The silicon nitride ceramics method that Holmium trioxide Praseodymium trioxide involved in the present invention is produced as additive pressureless sintering comprises the steps:
Step 1; Take by weighing Holmium trioxide Praseodymium trioxide and silicon nitride ceramics powder respectively; In planetary ball mill, change mixing 2 hours with PM 270～330, dispersion medium is an absolute ethyl alcohol, subsequently 60 ℃ of oven dry; Time is 2～3 hours, Holmium trioxide 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 Holmium trioxide is 3%～7%, and the weight percent of Praseodymium trioxide is 5%～8%, and the weight percent of silicon nitride is 85%～92%.
In the step 1, α-Si in the said silicon nitride
3N
4Content is greater than 90%.
In the step 1, said Holmium trioxide Praseodymium trioxide content is all 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 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
The Holmium trioxide Praseodymium trioxide is Ganzhou Jiarun novel material ltd, and silicon nitride powder is the M11 powder that German Starck company produces.Take by weighing 3% Holmium trioxide, 5% Praseodymium trioxide and 92% 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 3.62g/cm
3, folding strength is 681Mpa.
Claims (7)
1. the silicon nitride ceramics produced as additive pressureless sintering of a praseodymium holmium related Holmium trioxide Praseodymium trioxide of production technique of stablizing silicon nitride ceramics; Component and mass percentage content are: Holmium trioxide 3%～7%; Praseodymium trioxide 5%～8%, silicon nitride 85%～92%.3～6 microns of described Holmium trioxide granularities, 5～7 microns of Praseodymium trioxide granularities, 0.4～0.7 micron of silicon nitride granularity.
2. the silicon nitride ceramics method that the related Holmium trioxide Praseodymium trioxide of the production technique that a kind of praseodymium holmium according to claim 1 is stablized silicon nitride ceramics is produced as additive pressureless sintering comprises the steps:
Step 1; Take by weighing Holmium trioxide Praseodymium trioxide and silicon nitride ceramics powder respectively; In planetary ball mill, change mixing 2 hours with PM 270～330, dispersion medium is an absolute ethyl alcohol, subsequently 60 ℃ of oven dry; Time is 2～3 hours, Holmium trioxide 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. a kind of praseodymium holmium according to claim 2 is stablized the production technique of silicon nitride ceramics; The weight percent that it is characterized in that Holmium trioxide described in the step 1 is 3%～7%; The weight percent of Praseodymium trioxide is 5%～8%, and the weight percent of silicon nitride is 85%～92%.
4. a kind of praseodymium holmium according to claim 2 is stablized the production technique of silicon nitride ceramics, it is characterized in that in the step 1 α-Si in the said silicon nitride
3N
4Content is greater than 90%.
5. a kind of praseodymium holmium according to claim 2 is stablized the production technique of silicon nitride ceramics, it is characterized in that in the step 1, and content is all greater than 98% in the said Holmium trioxide Praseodymium trioxide.
6. a kind of praseodymium holmium according to claim 2 is stablized the production technique of silicon nitride ceramics, it is characterized in that in the step 3, and said nitrogen gas pressure is 1～2 normal atmosphere.
7. a kind of praseodymium holmium according to claim 2 is stablized the production technique of silicon nitride ceramics, it is characterized in that in the step 4, and said mechanical property is a folding strength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106009711A CN102531615A (en) | 2010-12-20 | 2010-12-20 | Process for producing silicon nitride ceramic stabilized by rare-earth praseodymium and holmium |
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| CN2010106009711A CN102531615A (en) | 2010-12-20 | 2010-12-20 | Process for producing silicon nitride ceramic stabilized by rare-earth praseodymium and holmium |
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| CN102531615A true CN102531615A (en) | 2012-07-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341206A (en) * | 2020-11-05 | 2021-02-09 | 衡阳凯新特种材料科技有限公司 | Forming method of rare earth praseodymium-holmium-stabilized silicon nitride ceramic |
-
2010
- 2010-12-20 CN CN2010106009711A patent/CN102531615A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341206A (en) * | 2020-11-05 | 2021-02-09 | 衡阳凯新特种材料科技有限公司 | Forming method of rare earth praseodymium-holmium-stabilized silicon nitride ceramic |
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Application publication date: 20120704 |