CN106495703B - A kind of preparation method of silicon nitride sealing ring - Google Patents

A kind of preparation method of silicon nitride sealing ring Download PDF

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CN106495703B
CN106495703B CN201610955910.4A CN201610955910A CN106495703B CN 106495703 B CN106495703 B CN 106495703B CN 201610955910 A CN201610955910 A CN 201610955910A CN 106495703 B CN106495703 B CN 106495703B
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silicon nitride
sealing ring
powder
dehydrated alcohol
preparation
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CN106495703A (en
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汪彩芬
徐俊
杨少青
白彬
王小英
岳映雷
朱彩强
苏尧
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China Nuclear Power Engineering Co Ltd
Institute of Materials of CAEP
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Abstract

The invention discloses a kind of preparation methods of silicon nitride sealing ring, comprising: (1) prepares raw material: silicon nitride powder, magnesia, aluminium oxide, yttrium oxide;(2) it adds the raw material into dehydrated alcohol, mixes, obtain silicon nitride composite powder slurry;(3) silicon nitride composite powder slurry is dried in vacuo, then crosses 80 meshes, obtains xeraphium;(4) glue is added and is mixed into xeraphium, then crossed 60 meshes, obtain silicon nitride pelletizing;(5) silicon nitride pelletizing is pressed and molded and silicon nitride ring billet body is made;(6) silicon nitride ring billet body is packed into graphite crucible, and is embedded to mixed powder, 1~3 hour is then kept the temperature under the conditions of nitrogen atmosphere, 1680~1740 DEG C and is sintered, silicon nitride sealing ring is made.Silicon nitride sealing ring relative density >=98% produced by the present invention, intensity > 650MPa, hardness (HRA) are 90~92, and fracture toughness is 4~6MPam1/2, very well satisfy the application of silicon nitride material in the market in sealing ring.

Description

A kind of preparation method of silicon nitride sealing ring
Technical field
The present invention relates to a kind of preparation methods of silicon nitride sealing ring.
Background technique
Silicon nitride ceramics is used due to its good mechanical property and excellent self-lubrication as sealing element.Currently, Domestic silicon nitride material is mainly prepared by reaction-sintered, hot pressing and HIP sintering technique.Product made from reaction-sintered contains There is increased number of stomata, relative density is less than 85%, and mechanical property is low, intensity is lower, only 150~350MPa.And hot pressing, heat Isostatic sintering not only needs expensive agglomerating plant and auxiliary consumptive material (such as jacket), but also is sintered (high temperature and pressure at high cost Required water, electricity, gas etc.), cause cost of goods manufactured high, seriously contained silicon nitride material in sealing ring answering in the market With.
Also, silicon nitride material self-diffusion coefficient is low, itself is sintered difficulty, and is extremely easy to decompose at high temperature, often Need high pressure could densified sintering product.
Therefore, it is necessary to which the new process of silicon nitride material high densification sintering can be completed under researching and developing a kind of low pressure.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of silicon nitride sealing ring, only need to be in 0.1MPa (atmospheric pressure Pressure), N2Atmosphere under can be completed silicon nitride material high densification sintering.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of silicon nitride sealing ring, comprising the following steps:
(1) by following weight ratio prepare raw material: silicon nitride powder 85~93%, magnesia 0.5~3%, aluminium oxide 3~7%, Yttrium oxide 3~8%;
(2) it adds the raw material into the dehydrated alcohol as powder decentralized medium, then mixes, be configured to solid concentration and exist 50~65% silicon nitride composite powder slurry;
(3) silicon nitride composite powder slurry is dried in vacuo, then crosses 80 meshes, obtains xeraphium;
(4) glue prepared in advance is added in the xeraphium to sieving and is mixed, then uniform 60 mesh of mistake, is nitrogenized Silicon pelletizing;The glue is made of binder and dehydrated alcohol, wherein and binder content is the 1~4% of xeraphium weight, Dehydrated alcohol content is the 12~20% of xeraphium weight;
(5) silicon nitride pelletizing is poured into sealing ring mold, is then pressed and molded under the pressure of 100~170MPa, made Obtain silicon nitride ring billet body;
(6) silicon nitride ring billet body is packed into graphite crucible, and is embedded to the mixed powder being made of additive, BN and silicon nitride, Then in normal pressure-sintered furnace, 1~3 hour being kept the temperature under the conditions of nitrogen atmosphere, 1680~1740 DEG C and is sintered, it is close that silicon nitride is made Seal ring;The additive, BN, desalination silicon account for 5~12%, 40~60% and the 28~55% of mixed powder weight respectively.
Further, in the step (2), raw material and dehydrated alcohol are mixed by the way of ball milling.
Preferably, ball, material ratio 2~3: 1 when the ball milling.
Preferably, the binder is polyethylene glycol, arbitrary one or two kinds of in polyvinyl alcohol carboxylic butyraldehyde.
Still further, silicon nitride composite powder slurry is put into vacuum oven, and in the step (3) in 85 DEG C Above temperature is dried in vacuo.
Specifically, magnesia, aluminium oxide and yttrium oxide group that the additive is 1~3: 2~5: 2~4 by weight ratio At.
Further, in the step (4), the preparation process of glue are as follows: pour into binder in dehydrated alcohol, and in 90 DEG C water bath condition under, be heated to binder and be completely dissolved with dehydrated alcohol.
Compared with prior art, the invention has the following advantages:
The present invention helps burning to make by addition sintering aid (magnesia, aluminium oxide and rare earth oxide) to what silicon nitride was sintered With effectively reducing the sintering temperature of silicon nitride densification, while the atmosphere being sintered by buried powder process adjustments effectively inhibits nitrogen The decomposition of SiClx at high temperature, so that densification sintering can be completed under atmospheric pressure kiln in entire silicon nitride material.Practice have shown that this The silicon nitride sealing ring of preparation is invented, not only performance indicator is much higher than reaction-sintered (silicon nitride sealing ring relative density obtained More than or equal to 98%, intensity is greater than 650MPa, and HRA hardness can reach 90~92, and fracture toughness can reach 4.5~6MPam1 /2), and since Parameter Conditions are more conventional, thus preparation cost is also far below hot pressing, HIP sintering technique.
Specific embodiment
Below with reference to embodiment, the invention will be further described, and mode of the invention includes but are not limited to following implementation Example.
The present invention provides a kind of novel silicon nitride sealing ring preparation processes, using silicon nitride powder as raw material, and are aided with Magnesia, aluminium oxide and yttrium oxide realize the high densification sintering of silicon nitride material as sintering aid.
Concrete technology flow process of the invention is as follows:
(1) by weight preparation raw material: silicon nitride powder 85~93%, magnesia 0.5~3%, aluminium oxide 3~7%, oxidation Yttrium 3~8%;
(2) it adds the raw material into the dehydrated alcohol as powder decentralized medium, then mixes, be configured to solid concentration and exist 50~65% silicon nitride composite powder slurry;The present embodiment is mixed raw material and dehydrated alcohol by the way of ball milling, and ball, material Than 2~3: 1;
(3) silicon nitride composite powder slurry is put into vacuum oven, is dried in vacuo under conditions of 85 DEG C or more, Then 80 meshes are crossed, xeraphium is obtained;
(4) glue prepared in advance is added in the xeraphium to sieving and is mixed, then uniform 60 mesh of mistake, is nitrogenized Silicon pelletizing;The glue is by binder (arbitrary one or two in polyethylene glycol, polyvinyl alcohol carboxylic butyraldehyde) and anhydrous second Alcohol composition, wherein binder content be xeraphium weight 1~4%, dehydrated alcohol content be xeraphium weight 12~ 20%;
(5) silicon nitride pelletizing is poured into sealing ring mold, is then pressed and molded under the pressure of 100~170MPa, made Obtain silicon nitride ring billet body;
(6) silicon nitride ring billet body is packed into graphite crucible, and being embedded to by additive (is 1~3: 2~5: 2~4 by weight ratio Magnesia, aluminium oxide and yttrium oxide composition), BN and silicon nitride composition mixed powder, then in normal pressure-sintered furnace, in nitrogen Atmosphere keeps the temperature 1~3 hour under the conditions of 1680~1740 DEG C and is sintered, and silicon nitride sealing ring is made;The additive, BN, nitridation Silicon accounts for 5~12%, 40~60% and the 28~55% of mixed powder weight respectively.
The silicon nitride sealing ring relative density that the present invention is prepared is greater than or is equal to 98%, and intensity is greater than 650MPa, HRA Hardness can reach 90~92, and fracture toughness can reach 4.5~6MPam1/2.Below with several examples to effect of the invention into Row illustrates.
Example 1
Silicon nitride powder, magnesia, aluminium oxide, yttrium oxide weight ratio be respectively 93%, 3.5%, 0.5% and 3%, by four Person forms mixed powder, then according to mixed powder: abrading-ball: dehydrated alcohol=1: 2.5: 0.6 weight ratio configuration abrading-ball and anhydrous second Alcohol, and above-mentioned mixed-powder, abrading-ball and dehydrated alcohol are poured into ball grinder, ball milling 48 hours, obtain the compound slurry of silicon nitride Material.
Then, silicon nitride composite powder slurry is dried under conditions of 90 DEG C in vacuum drying oven, and crosses 80 meshes.It connects , PVB is weighed by the mixed powder weight ratio 1% of drying sieving, weighs anhydrous second by the mixed powder weight ratio 16% of drying sieving Alcohol, and load weighted PVB is poured into dehydrated alcohol, it is heated to PVB under 90 DEG C of water bath conditions and is completely dissolved with dehydrated alcohol, Colloidal sol is made.
Glue is poured into the mixed powder of drying sieving, hand mix uniformly crosses 60 meshes afterwards, obtains silicon nitride pelletizing, so After pour into sealing ring mold, in 170MPa be pressed and molded be made silicon nitride sealing ring green body.
Finally, above-mentioned silicon nitride sealing ring green body is packed into crucible, and inserts buried powder (buried powder composition be weight ratio is 1% Magnesia+2% aluminium oxide+2% yttrium oxide+40% BN+55% Si3N4Mixed powder), then 1735 DEG C, often Pressure, N2It under atmospheric condition, keeps the temperature 2 hours and is sintered, silicon nitride sealing ring is made.
Silicon nitride sealing ring made from this example, relative density 98.6%, intensity 700MPa, hardness (HRA) are 92, fracture toughness 5.4MPam1/2
Example 2
Silicon nitride powder, magnesia, aluminium oxide, yttrium oxide weight ratio be respectively 90%, 5.5%, 1% and 3.5%, by four Person forms mixed powder, then according to mixed powder: abrading-ball: dehydrated alcohol=1: 3: 0.9 weight ratio configuration abrading-ball and dehydrated alcohol, And pour into above-mentioned mixed-powder, abrading-ball and dehydrated alcohol in ball grinder, ball milling 56 hours, obtain silicon nitride composite powder slurry.
Then, silicon nitride composite powder slurry is dried under conditions of 90 DEG C in vacuum drying oven, and crosses 80 meshes.It connects , PVB, PEG are weighed respectively by the mixed powder weight ratio 1% of drying sieving, are claimed by the mixed powder weight ratio 16% of drying sieving Measure dehydrated alcohol, and load weighted PVB, PEG poured into dehydrated alcohol, be heated under 90 DEG C of water bath conditions PVB, PEG with Dehydrated alcohol is completely dissolved, and colloidal sol is made.
Glue is poured into the mixed powder of drying sieving, hand mix uniformly crosses 60 meshes afterwards, obtains silicon nitride pelletizing, so After pour into sealing ring mold, in 150MPa be pressed and molded be made silicon nitride sealing ring green body.
Finally, above-mentioned silicon nitride sealing ring green body is packed into crucible, and inserts buried powder (buried powder composition be weight ratio is 2% Magnesia+4% aluminium oxide+4% yttrium oxide+50% BN+40% Si3N4Mixed powder), then 1720 DEG C, often Pressure, N2It under atmospheric condition, keeps the temperature 3 hours and is sintered, silicon nitride sealing ring is made.
Silicon nitride sealing ring made from this example, relative density 98.6%, intensity 740MPa, hardness (HRA) are 91, fracture toughness 6.0MPam1/2
Example 3
Silicon nitride powder, magnesia, aluminium oxide, yttrium oxide weight ratio be respectively 85%, 7.5%, 2.5% and 5%, by four Person forms mixed powder, then according to mixed powder: abrading-ball: dehydrated alcohol=1: 2: 1 weight ratio configuration abrading-ball and dehydrated alcohol, and Above-mentioned mixed-powder, abrading-ball and dehydrated alcohol are poured into ball grinder, ball milling 90 hours, obtains silicon nitride composite powder slurry.
Then, silicon nitride composite powder slurry is dried under conditions of 90 DEG C in vacuum drying oven, and crosses 80 meshes.It connects , PEG is weighed by the mixed powder weight ratio 3% of drying sieving, weighs anhydrous second by the mixed powder weight ratio 20% of drying sieving Alcohol, and load weighted PEG is poured into dehydrated alcohol, it is heated to PEG under 90 DEG C of water bath conditions and is completely dissolved with dehydrated alcohol, Colloidal sol is made.
Glue is poured into the mixed powder of drying sieving, hand mix uniformly crosses 60 meshes afterwards, obtains silicon nitride pelletizing, so After pour into sealing ring mold, in 120MPa be pressed and molded be made silicon nitride sealing ring green body.
Finally, above-mentioned silicon nitride sealing ring green body is packed into crucible, and inserts buried powder (buried powder composition be weight ratio is 3% Magnesia+5% aluminium oxide+4% yttrium oxide+60% BN+28% Si3N4Mixed powder), then 1680 DEG C, often Pressure, N2It under atmospheric condition, keeps the temperature 1 hour and is sintered, silicon nitride sealing ring is made.
Silicon nitride sealing ring made from this example, relative density 98.2%, intensity 675MPa, hardness (HRA) are 91, fracture toughness 4.7MPam1/2
The present invention compares for prior art, not only low in cost, but also process flow is simple, high-efficient, in 0.1MPa (atmospheric pressure), N2Atmosphere under can be completed silicon nitride material high densification sintering.The present invention is reasonable by raw material It selects and proportion has well solved silicon nitride material and be difficult to realize asking for high densification sintering in conjunction with the sintering process of design Topic, has given full play to the characteristic of its mechanical property and self-lubricating, greatly meets silicon nitride material in sealing ring in the market Using.Therefore, the technology of the present invention progress is obvious, has substantive distinguishing features outstanding and significant progress.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention Enclose, it is all in body design thought of the invention and mentally make have no the change of essential meaning or polishing, solved Technical problem is still consistent with the present invention, should all be included within protection scope of the present invention.

Claims (5)

1. a kind of preparation method of silicon nitride sealing ring, which comprises the following steps:
(1) prepare raw material: silicon nitride powder 85~93%, magnesia 0.5~3%, aluminium oxide 3~7%, yttrium oxide 3 by following weight ratio ~8%;
(2) add the raw material into the dehydrated alcohol as powder decentralized medium, then mix, be configured to solid concentration 50~ 65% silicon nitride composite powder slurry;
(3) silicon nitride composite powder slurry is dried in vacuo, then crosses 80 meshes, obtains xeraphium;
(4) glue prepared in advance is added in the xeraphium to sieving and is mixed, then uniform 60 mesh of mistake, obtains silicon nitride and make Grain powder;The glue is made of binder and dehydrated alcohol, wherein binder content is the 1~4% of xeraphium weight, anhydrous second Alcohol content is the 12~20% of xeraphium weight;
(5) silicon nitride pelletizing is poured into sealing ring mold, is then pressed and molded under the pressure of 100~170MPa, nitrogen is made SiClx ring billet body;
(6) silicon nitride ring billet body is packed into graphite crucible, and is embedded to the mixed powder being made of additive, BN and silicon nitride, then In normal pressure-sintered furnace, 1~3 hour being kept the temperature under the conditions of nitrogen atmosphere, 1680~1740 DEG C and is sintered, silicon nitride sealing is made Ring;The additive, BN, silicon nitride account for 5~12%, 40~60% and the 28~55% of mixed powder weight respectively;
The binder is polyethylene glycol, arbitrary one or two kinds of in polyvinyl alcohol carboxylic butyraldehyde;
The additive is made of magnesia, aluminium oxide and the yttrium oxide that weight ratio is 1~3: 2~5: 2~4.
2. a kind of preparation method of silicon nitride sealing ring according to claim 1, which is characterized in that in the step (2), Raw material and dehydrated alcohol are mixed by the way of ball milling.
3. a kind of preparation method of silicon nitride sealing ring according to claim 2, which is characterized in that when the ball milling Ball, material ratio 2~3: 1.
4. a kind of preparation method of silicon nitride sealing ring according to claim 3, which is characterized in that in the step (3), Silicon nitride composite powder slurry is put into vacuum oven, and is dried in vacuo in 85 DEG C or more of temperature.
5. a kind of preparation method of silicon nitride sealing ring according to any one of claims 1-4, which is characterized in that described In step (4), the preparation process of glue are as follows: binder is poured into dehydrated alcohol, and under 90 DEG C of water bath condition, is heated to gluing Knot agent is completely dissolved with dehydrated alcohol.
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