CN105801128A - Silicon nitride ceramic and method for preparing same - Google Patents

Silicon nitride ceramic and method for preparing same Download PDF

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CN105801128A
CN105801128A CN201610386958.8A CN201610386958A CN105801128A CN 105801128 A CN105801128 A CN 105801128A CN 201610386958 A CN201610386958 A CN 201610386958A CN 105801128 A CN105801128 A CN 105801128A
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silicon nitride
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nitride ceramics
organic solvent
oxide
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吴依妮
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Abstract

The invention provides a silicon nitride ceramic and a method for preparing the same, and relates to the field of ceramic preparation. The silicon nitride ceramic mainly comprises, by weight, 80-95 parts of alpha-Si3N4, 10-30 parts of silicon carbide, 0.5-5 parts of aluminum oxide, 0.5-5 parts of magnesium oxide, 2-10 parts of rare-earth metal oxide, 10-15 parts of binders, 7-14 parts of surfactants, 15-20 parts of deionized water, 16-24 parts of organic solvents, 1-5 parts of zirconium oxide and 1-5 parts of auxiliaries. The silicon nitride ceramic and the method have the advantages that the silicon nitride ceramic prepared by the aid of the method is good in toughness, high in hardness and strength and low in density and is corrosion-resistant and high-temperature-resistant, and accordingly the silicon nitride ceramic and the method are wide in application range.

Description

A kind of silicon nitride ceramics and preparation method thereof
Technical field
The invention belongs to field of ceramic preparation, concretely relate to a kind of silicon nitride ceramics and preparation method thereof.
Background technology
Non-shrinking inorganic material when silicon nitride ceramics is a kind of sintering.Silicon nitride ceramics is with its high rigidity, low-density, height The plurality of advantages such as intensity, corrosion-resistant, resistance to elevated temperatures is good, are widely studied and applied, and are mainly used in high temperature, burn into grinds by force On the extreme environments such as damage and some electronic devices and components, such as ceramic engine turbine, cast aluminium crucible, cutter, heat-radiating substrate, bearing Ball etc..But, the fragility of ceramic material significantly limit its application in these areas.It is thus desirable to research has concurrently tough Property good with high rigidity, high intensity, low-density, the ceramic material of the excellent performance such as corrosion-resistant, high temperature resistant, apply model widening it Enclose.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides a kind of silicon nitride ceramics and preparation method thereof.To improve existing nitrogen The problem of SiClx ceramics toughness difference.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of silicon nitride ceramics, mainly includes following raw material, by parts by weight meter: α-Si3N4 80-95 part, carborundum 10-30 Part, aluminium oxide 0.5-5 part, magnesium oxide 0.5-5 part, rare-earth oxide 2-10 part, binding agent 10-15 part, surfactant 7-14 part, deionized water 15-20 part, organic solvent 16-24 part, zirconium oxide 1-5 part, auxiliary agent 1-5 part.
Preferably, in the preferred embodiment, described rare-earth oxide is Yb2O3、Lu2O3、Sc2O3、 Y2O3、La2O3、Ce2O3、Pr2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3And Tm2O3 In at least two composition.
Preferably, in the preferred embodiment, described auxiliary agent is in terms of parts by weight, by Kaolin 3-5 part, nanometer Boron fibre 0.6-0.9 part, nano-sized carbon 0.3-0.5 part, silane coupler 0.4-0.8 part, Polyethylene Glycol 0.2-0.5 part, deionization Water 6-10 part forms.
Preferably, in the preferred embodiment, during described organic solvent is dimethylbenzene, acetone or dehydrated alcohol A kind of.
Present invention also offers the preparation method of a kind of silicon nitride ceramics, comprise the following steps:
(1) described α-Si is weighed by proportioning3N4, described carborundum, described aluminium oxide, described magnesium oxide, described rare earth metal oxygen Compound crosses 80-200 mesh sieve, then adds in described organic solvent and mix homogeneously by each component, obtains slurry；
(2) at 105-135 DEG C, being dried the described slurry extremely mass percent of organic solvent described in described slurry is 1.5- 2.5%, obtain mixed powder；
(3) go described in described mixed powder, described binding agent, described surfactant, described zirconium oxide, the addition of described auxiliary agent In ionized water, sending in ball mill, in 120-160r/min ball milling 21-25 hour, being washed to pH value was 7-9, filters, To filter cake；
(4) described filter cake is carried out successively dry-pressing formed and hip moulding, obtain green compact；
(5) described green compact are sintered in argon, and sintering temperature is 1600-2100 DEG C, and sintering time is 30-160min, stops Only it is cooled to 20-35 DEG C after heating, obtains silicon nitride ceramics.
Preferably, in the preferred embodiment, the gross mass of each component described in step (1) and organic solvent Mass ratio is 1:1-5.
Preferably, in the preferred embodiment, described argon can be replaced the mass percent of nitrogen or hydrogen Nitrogen less than 10% and the mixed gas of hydrogen.
Preferably, in the preferred embodiment, described sintering temperature is warming up to the speed of 60-80 DEG C/min 1600℃-2100℃。
Beneficial effects of the present invention: silicon nitride ceramics provided by the present invention not only has high rigidity, high intensity, low close Degree, the performance such as corrosion-resistant, high temperature resistant, also have high tenacity concurrently, widened its range of application.The present invention is by adding rare earth metal oxygen Compound makes silicon nitride modification, enhances its toughness.Through heat and other static pressuring processes, prepared silicon nitride ceramics intensity is the highest, is generation One of material the hardest in boundary, puts in cold water after the silicon nitride of hot pressed sintering is heated to l000 DEG C and also will not rupture.Logical Cross and make used additives, by increasing capacitance it is possible to increase surface smoothness, wearability and the thermostability of pottery.
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1:
A kind of silicon nitride ceramics, mainly includes following raw material, by parts by weight meter: α-Si3N4 80 parts, carborundum 10 parts, oxidation 0.5 part of aluminum, magnesium oxide 0.5 part, rare-earth oxide 2 parts, binding agent 10 parts, 7 parts of surfactant, deionized water 15 parts, Organic solvent 16 parts, zirconium oxide 1 part, auxiliary agent 1 part.
Rare-earth oxide is Yb2O3、Y2O3、La2O3、Ce2O3。
Auxiliary agent is in terms of parts by weight, by Kaolin 3 parts, nanometer boron fibre 0.6 part, nano-sized carbon 0.3 part, silane coupler 0.4 part, Polyethylene Glycol 0.2 part, deionized water 6 parts composition.
Organic solvent is dimethylbenzene.
The present embodiment additionally provides the preparation method of a kind of silicon nitride ceramics, comprises the following steps:
(1) α-Si is weighed by proportioning3N4, carborundum, aluminium oxide, magnesium oxide, rare-earth oxide cross 80 mesh sieves, then will be each Component adds in organic solvent and mix homogeneously, obtains slurry；
(2) at 105 DEG C, being dried slurry is 1.5% to the mass percent of organic solvent in slurry, obtains mixed powder；
(3) mixed powder, binding agent, surfactant, zirconium oxide, auxiliary agent are added in deionized water, send in ball mill, in 120r/min ball milling 21 hours, being washed to pH value is 7, filters, obtains filter cake；
(4) filter cake is carried out successively dry-pressing formed and hip moulding, obtain green compact；
(5) green compact are sintered in argon, and sintering temperature is 1600 DEG C, and sintering time is 30min, cool down after stopping heating To 20 DEG C, obtain silicon nitride ceramics.
The gross mass of each component described in step (1) and the mass ratio of organic solvent are 1:1.
Argon can be replaced nitrogen.
Sintering temperature is warming up to 1600 DEG C with the speed of 60 DEG C/min.
Embodiment 2:
A kind of silicon nitride ceramics, mainly includes following raw material, by parts by weight meter: α-Si3N495 parts, carborundum 30 parts, oxidation 5 parts of aluminum, magnesium oxide 5 parts, rare-earth oxide 10 parts, binding agent 15 parts, 14 parts of surfactant, deionized water 20 parts, have Machine solvent 24 parts, zirconium oxide 5 parts, auxiliary agent 5 parts.
Rare-earth oxide is Yb2O3、Y2O3。
Auxiliary agent is in terms of parts by weight, by Kaolin 5 parts, nanometer boron fibre 0.9 part, nano-sized carbon 0.5 part, silane coupler 0.8 part, Polyethylene Glycol 0.5, deionized water 10 parts composition.
Organic solvent is acetone.
The present embodiment additionally provides the preparation method of a kind of silicon nitride ceramics, comprises the following steps:
(1) α-Si is weighed by proportioning3N4, carborundum, aluminium oxide, magnesium oxide, rare-earth oxide cross 200 mesh sieves, then will Each component adds in organic solvent and mix homogeneously, obtains slurry；
(2) at 135 DEG C, being dried slurry is 2.5% to the mass percent of organic solvent in slurry, obtains mixed powder；
(3) mixed powder, binding agent, surfactant, zirconium oxide, auxiliary agent are added in deionized water, send in ball mill, in 160r/min ball milling 25 hours, being washed to pH value is 9, filters, obtains filter cake；
(4) filter cake is carried out successively dry-pressing formed and hip moulding, obtain green compact；
(5) green compact are sintered in argon, and sintering temperature is 2100 DEG C, and sintering time is 160min, cool down after stopping heating To 35 DEG C, obtain silicon nitride ceramics.
The gross mass of each component described in step (1) and the mass ratio of organic solvent are 1:1-5.
Argon can be replaced the mixed gas of the mass percent of the hydrogen nitrogen less than 10% and hydrogen.
Sintering temperature is warming up to 2100 DEG C with the speed of 80 DEG C/min.
Embodiment 3:
A kind of silicon nitride ceramics, mainly includes following raw material, by parts by weight meter: α-Si3N4 87 parts, carborundum 20 parts, oxidation 2.7 parts of aluminum, magnesium oxide 2.7 parts, rare-earth oxide 6 parts, binding agent 12.5 parts, 10.5 parts of surfactant, deionized water 17.5 parts, organic solvent 20 parts, zirconium oxide 3 parts, auxiliary agent 3 parts.
Rare-earth oxide is Yb2O3、Ce2O3。
Auxiliary agent is in terms of parts by weight, by Kaolin 4 parts, nanometer boron fibre 0.75 part, nano-sized carbon 0.4 part, silane coupler 0.6 part, Polyethylene Glycol 0.35, deionized water 8 parts composition.
Organic solvent is dimethylbenzene.
The present embodiment additionally provides the preparation method of a kind of silicon nitride ceramics, comprises the following steps:
(1) α-Si is weighed by proportioning3N4, carborundum, aluminium oxide, magnesium oxide, rare-earth oxide cross 140 mesh sieves, then will Each component adds in organic solvent and mix homogeneously, obtains slurry；
(2) at 120 DEG C, being dried slurry is 2% to the mass percent of organic solvent in slurry, obtains mixed powder；
(3) mixed powder, binding agent, surfactant, zirconium oxide, auxiliary agent are added in deionized water, send in ball mill, in 140r/min ball milling 23 hours, being washed to pH value is 8, filters, obtains filter cake；
(4) filter cake is carried out successively dry-pressing formed and hip moulding, obtain green compact；
(5) green compact are sintered in argon, and sintering temperature is 1900 DEG C, and sintering time is 95min, cool down after stopping heating To 27 DEG C, obtain silicon nitride ceramics.
The gross mass of each component described in step (1) and the mass ratio of organic solvent are 1:3.
Argon can be replaced the mixed gas of the mass percent nitrogen less than 10% and hydrogen.
Sintering temperature is warming up to 1900 DEG C with the speed of 70 DEG C/min.
The Vickers hardness of silicon nitride ceramics, wear-out life, the fracture toughness that prepare embodiment 1-3 are tested, test Result is as shown in table 1:
Table 1 embodiment 1-3 the performance test results

Claims (8)

1. a silicon nitride ceramics, it is characterised in that mainly include following raw material, by parts by weight meter: α-Si3N4 80-95 part, Carborundum 10-30 part, aluminium oxide 0.5-5 part, magnesium oxide 0.5-5 part, rare-earth oxide 2-10 part, binding agent 10-15 part, Surfactant 7-14 part, deionized water 15-20 part, organic solvent 16-24 part, zirconium oxide 1-5 part, auxiliary agent 1-5 part.
Silicon nitride ceramics the most according to claim 1, it is characterised in that: described rare-earth oxide is Yb2O3、Lu2O3、 Sc2O3、Y2O3、La2O3、Ce2O3、Pr2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3With Tm2O3In at least two composition.
Silicon nitride ceramics the most according to claim 1, it is characterised in that: described auxiliary agent is in terms of parts by weight, by Kaolin 3-5 part, nanometer boron fibre 0.6-0.9 part, nano-sized carbon 0.3-0.5 part, silane coupler 0.4-0.8 part, Polyethylene Glycol 0.2- 0.5 part, deionized water 6-10 part composition.
Silicon nitride ceramics the most according to claim 1, it is characterised in that: described organic solvent is dimethylbenzene, acetone or nothing One in water-ethanol.
5. the preparation method of the silicon nitride ceramics as described in any one of claim 1-4, it is characterised in that include following step Rapid:
(1) described α-Si is weighed by proportioning3N4, described carborundum, described aluminium oxide, described magnesium oxide, described rare earth metal oxidation Thing crosses 80-200 mesh sieve, then adds in described organic solvent and mix homogeneously by each component, obtains slurry；
(2) at 105-135 DEG C, being dried the described slurry extremely mass percent of organic solvent described in described slurry is 1.5- 2.5%, obtain mixed powder；
(3) go described in described mixed powder, described binding agent, described surfactant, described zirconium oxide, the addition of described auxiliary agent In ionized water, sending in ball mill, in 120-160r/min ball milling 21-25 hour, being washed to pH value was 7-9, filters, To filter cake；
(4) described filter cake is carried out successively dry-pressing formed and hip moulding, obtain green compact；
(5) described green compact are sintered in argon, and sintering temperature is 1600-2100 DEG C, and sintering time is 30-160min, stops Only it is cooled to 20-35 DEG C after heating, obtains silicon nitride ceramics.
The preparation method of silicon nitride ceramics the most according to claim 5, it is characterised in that: each component described in step (1) The mass ratio of gross mass and organic solvent be 1:1-5.
The preparation method of silicon nitride ceramics the most according to claim 5, it is characterised in that: described argon can be replaced nitrogen Or the mass percent of hydrogen is less than the nitrogen of 10% and the mixed gas of hydrogen.
The preparation method of silicon nitride ceramics the most according to claim 5, it is characterised in that: described sintering temperature is with 60-80 DEG C/speed of min is warming up to 1600 DEG C-2100 DEG C.
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