CN102557651A - Preparation process of dysprosium oxide reinforced silicon nitride - Google Patents
Preparation process of dysprosium oxide reinforced silicon nitride Download PDFInfo
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- CN102557651A CN102557651A CN2010106013670A CN201010601367A CN102557651A CN 102557651 A CN102557651 A CN 102557651A CN 2010106013670 A CN2010106013670 A CN 2010106013670A CN 201010601367 A CN201010601367 A CN 201010601367A CN 102557651 A CN102557651 A CN 102557651A
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- silicon nitride
- dysprosium oxide
- strengthened
- preparation technology
- holmium trioxide
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Abstract
The invention relates to the technical field of a ceramic material, in particular to a method for producing a high-performance silicon nitride (Si3N4) ceramic by pressureless sintering of holimium oxide and dysprosium oxide as additives. The ceramic material comprises the following components in percentage by mass: 3-7% of holimium oxide, 5-8% of dysprosium oxide and 85-92% of silicon nitride. The aim of the invention is to overcome the defects in the prior art and provide a method for producing a high-performance silicon nitride ceramic by pressureless sintering of holimium oxide and dysprosium oxide as additives. The method can be widely applied to parts manufacturing in the fields of chemical engineering, 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 dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide involved in the present invention is produced as additive pressureless sintering, component and mass percentage content are: Holmium trioxide 3%～7%, dysprosium oxide 5%～8%, silicon nitride 85%～92%.
3～6 microns of described Holmium trioxide granularities, 5～7 microns of dysprosium oxide granularities, 0.4～0.7 micron of silicon nitride granularity.
The silicon nitride ceramics method that Holmium trioxide dysprosium oxide involved in the present invention is produced as additive pressureless sintering comprises the steps:
Step 1; Take by weighing Holmium trioxide dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide 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 dysprosium oxide 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% dysprosium oxide 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 3.40g/cm
3, folding strength is 672Mpa.
Claims (7)
1. the silicon nitride ceramics produced as additive pressureless sintering of the related Holmium trioxide dysprosium oxide of silicon nitride preparation technology strengthened of a dysprosium oxide, component and mass percentage content are: Holmium trioxide 3%～7%, dysprosium oxide 5%～8%, silicon nitride 85%～92%.3～6 microns of described Holmium trioxide granularities, 5～7 microns of dysprosium oxide granularities, 0.4～0.7 micron of silicon nitride granularity.
2. the silicon nitride ceramics method that the related Holmium trioxide dysprosium oxide of the silicon nitride preparation technology that a kind of dysprosium oxide according to claim 1 is strengthened is produced as additive pressureless sintering comprises the steps:
Step 1; Take by weighing Holmium trioxide dysprosium oxide 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 dysprosium oxide 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 silicon nitride preparation technology that a kind of dysprosium oxide according to claim 2 is strengthened; The weight percent that it is characterized in that Holmium trioxide described in the step 1 is 3%～7%; The weight percent of dysprosium oxide is 5%～8%, and the weight percent of silicon nitride is 85%～92%.
4. the silicon nitride preparation technology that a kind of dysprosium oxide according to claim 2 is strengthened is characterized in that in the step 1 α-Si in the said silicon nitride
3N
4Content is greater than 90%.
5. the silicon nitride preparation technology that a kind of dysprosium oxide according to claim 2 is strengthened is characterized in that in the step 1 that content is all greater than 98% in the said Holmium trioxide dysprosium oxide.
6. the silicon nitride preparation technology that a kind of dysprosium oxide according to claim 2 is strengthened is characterized in that in the step 3 that said nitrogen gas pressure is 1～2 normal atmosphere.
7. the silicon nitride preparation technology that a kind of dysprosium oxide according to claim 2 is strengthened 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 |
|---|---|---|---|
| CN2010106013670A CN102557651A (en) | 2010-12-20 | 2010-12-20 | Preparation process of dysprosium oxide reinforced silicon nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106013670A CN102557651A (en) | 2010-12-20 | 2010-12-20 | Preparation process of dysprosium oxide reinforced silicon nitride |
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|---|---|
| CN102557651A true CN102557651A (en) | 2012-07-11 |
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|---|---|---|---|
| CN2010106013670A Pending CN102557651A (en) | 2010-12-20 | 2010-12-20 | Preparation process of dysprosium oxide reinforced silicon nitride |
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|---|---|
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2010
- 2010-12-20 CN CN2010106013670A patent/CN102557651A/en active Pending
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Application publication date: 20120711 |