CN102557658A - Method for producing nano holmium oxide-doped thulium oxide-stabilized silicon nitride - Google Patents
Method for producing nano holmium oxide-doped thulium oxide-stabilized silicon nitride Download PDFInfo
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- CN102557658A CN102557658A CN2010106209012A CN201010620901A CN102557658A CN 102557658 A CN102557658 A CN 102557658A CN 2010106209012 A CN2010106209012 A CN 2010106209012A CN 201010620901 A CN201010620901 A CN 201010620901A CN 102557658 A CN102557658 A CN 102557658A
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Abstract
The invention relates to the technical field of ceramic material, particularly to a method for producing high-performance silicon nitride (Si3N4) ceramic through pressureless sintering by using holmium oxide and thulium oxide as additives. The silicon nitride ceramic comprises the following components in percentage by mass: 3-7% of holmium oxide, 5-8% of thulium oxide, and 85-92% of silicon nitride. For overcoming the shortages in the prior art, the intention provides a method for producing high-performance silicon nitride ceramic through pressureless sintering by using holmium oxide and thulium oxide as additives, and the method can be widely used for preparing components and parts in the fields of chemical industry, machinery, metallurgy, aerospace, etc.
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 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 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 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 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 trioxide involved in the present invention is produced as additive pressureless sintering, component and mass percentage content are: Holmium trioxide 3%～7%, trioxide 5%～8%, silicon nitride 85%～92%.
3～6 microns of described Holmium trioxide granularities, 5～7 microns of trioxide granularities, 0.4～0.7 micron of silicon nitride granularity.
The silicon nitride ceramics method that Holmium trioxide trioxide involved in the present invention is produced as additive pressureless sintering comprises the steps:
Step 1; Take by weighing Holmium trioxide 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 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 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 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 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 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% 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 3.43g/cm
3, folding strength is 699Mpa.
Claims (7)
1. the silicon nitride ceramics that the related Holmium trioxide trioxide of the preparation method that nano oxidized holmium doping trioxide is stablized silicon nitride is produced as additive pressureless sintering; Component and mass percentage content are: Holmium trioxide 3%～7%; Trioxide 5%～8%, silicon nitride 85%～92%.3～6 microns of described Holmium trioxide granularities, 5～7 microns of trioxide granularities, 0.4～0.7 micron of silicon nitride granularity.
2. the silicon nitride ceramics method that the related Holmium trioxide trioxide of the preparation method that nano oxidized holmium doping trioxide according to claim 1 is stablized silicon nitride is produced as additive pressureless sintering comprises the steps:
Step 1; Take by weighing Holmium trioxide 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 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. nano oxidized holmium doping trioxide according to claim 2 is stablized the preparation method of silicon nitride; The weight percent that it is characterized in that Holmium trioxide described in the step 1 is 3%～7%; The weight percent of trioxide is 5%～8%, and the weight percent of silicon nitride is 85%～92%.
4. nano oxidized holmium doping trioxide according to claim 2 is stablized the preparation method of silicon nitride, it is characterized in that in the step 1 α-Si in the said silicon nitride
3N
4Content is greater than 90%.
5. nano oxidized holmium doping trioxide according to claim 2 is stablized the preparation method of silicon nitride, it is characterized in that in the step 1, and content is all greater than 98% in the said Holmium trioxide trioxide.
6. nano oxidized holmium doping trioxide according to claim 2 is stablized the preparation method of silicon nitride, it is characterized in that in the step 3, and said nitrogen gas pressure is 1～2 normal atmosphere.
7. nano oxidized holmium doping trioxide according to claim 2 is stablized the preparation method of silicon nitride, 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 |
|---|---|---|---|
| CN2010106209012A CN102557658A (en) | 2010-12-29 | 2010-12-29 | Method for producing nano holmium oxide-doped thulium oxide-stabilized silicon nitride |
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| CN2010106209012A CN102557658A (en) | 2010-12-29 | 2010-12-29 | Method for producing nano holmium oxide-doped thulium oxide-stabilized silicon nitride |
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| CN102557658A true CN102557658A (en) | 2012-07-11 |
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| CN2010106209012A Pending CN102557658A (en) | 2010-12-29 | 2010-12-29 | Method for producing nano holmium oxide-doped thulium oxide-stabilized silicon nitride |
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Application publication date: 20120711 |