CN108409336A - Silicon nitride ceramics and preparation method thereof - Google Patents
Silicon nitride ceramics and preparation method thereof Download PDFInfo
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Abstract
Silicon nitride ceramics and preparation method thereof belongs to ceramic material field.Preparation method includes：Raw material is mixed and dried using organic solvent, obtain ceramic powder, raw material includes silica flour, alpha silicon nitride, beta silicon nitride, boron nitride nano-tube, silicon carbide whisker, metal oxide and rare earth oxide, and the content of organic solvent is 5 8wt% in ceramic powder.Ceramic powder is pressed into biscuit of ceramics.Biscuit of ceramics is subjected to one-stage sintering under the conditions of 0.1 0.3MPa of nitrogen pressure, 200 300 DEG C of temperature；Then bis sintering is carried out under the conditions of 0.1 0.3Mpa of nitrogen pressure, 1,400 1500 DEG C of temperature；Finally three-stage sintering is carried out under the conditions of 1.5 2Mpa of nitrogen pressure, 1,700 1800 DEG C of temperature.Its is simple to operate, and silicon nitride ceramics obtained has the features such as good toughness, bending strength are high and cracking resistance is good.
Description
Technical field
The present invention relates to ceramic material fields, and more particularly to a kind of silicon nitride ceramics and preparation method thereof.
Background technology
Silicon nitride ceramics due to have many advantages, such as it is high than by force, it is Gao Bimo, high temperature resistant, anti-oxidant and wear-resistant, in high temperature, height
There is special use value in fast, strong corrosive medium working environment, thermal conductivity is good, and thermal shock resistance is strong, and dielectric
Constant and dielectric loss are low, have good frequency electromagnetic waves through performance, make it have the foreground of being widely applied.
Silicon nitride positioning pin is a kind of important silicon nitride ceramics structural member, is typically used in metal nut being welded to gold
It is mainly excellent using silicon nitride high intensity, wear-resistant, resistance to molten metal corrosion and insulating properties etc. on the elaborate position for belonging to plate
Performance.
But with the rapid development of science and technology, the weakness that silicon nitride ceramics brittleness is big, toughness is low is also increasingly by people
Attention, in practical applications the mechanical property of silicon nitride ceramics need to be further improved.
In view of this, special propose the application.
Invention content
It is simple to operate the purpose of the present invention is to provide a kind of preparation method of silicon nitride ceramics, nitrogen obtained
SiClx ceramics have the features such as good toughness, bending strength are high and cracking resistance is good.
Another object of the present invention is to provide a kind of silicon nitride ceramics, and it is high and anti-to have good toughness, bending strength
The features such as splitting excellent performance.
The present invention solves its technical problem using following technical scheme to realize.
The present invention proposes a kind of preparation method of silicon nitride ceramics, including：
Raw material is mixed and dried using organic solvent, ceramic powder is obtained, raw material includes silica flour, α-siliconnitride, β-nitrogen
SiClx, boron nitride nano-tube, silicon carbide whisker, metal oxide and rare earth oxide, organic solvent contains in ceramic powder
Amount is 5-8wt%.
Ceramic powder is pressed into biscuit of ceramics.
Biscuit of ceramics is subjected to one-stage sintering under the conditions of nitrogen pressure 0.1-0.3MPa, 200-300 DEG C of temperature；Then exist
Bis sintering is carried out under the conditions of nitrogen pressure 0.1-0.3Mpa, 1400-1500 DEG C of temperature；Finally nitrogen pressure 1.5-2Mpa,
Three-stage sintering is carried out under the conditions of 1700-1800 DEG C of temperature.
The present invention proposes a kind of silicon nitride ceramics, is made by above-mentioned preparation method.
The advantageous effect of the embodiment of the present invention is：
The preparation method of silicon nitride ceramics provided by the invention uses the compound of silica flour and α-siliconnitride and beta-silicon nitride
System is sintered, and using α-siliconnitride as major matrix material, silica flour nitrogenizes generation between being distributed evenly in α-siliconnitride
Silicon nitride is conducive to the consistency for improving silicon nitride ceramics；α-siliconnitride can generate channel of nitrogen, improve the nitriding rate of silica flour,
Improve the structure of tissue；The silicon nitride that beta-silicon nitride induces α-siliconnitride and silica flour to generate occurs to turn to the crystal form of beta-silicon nitride
Become, to increase product consistency and mechanical strength.On this basis, boron nitride nano-tube, silicon carbide whisker, one side energy are introduced
The bonding strength and tight ness rating between the silicon nitride that α-siliconnitride and silica flour generate enough are improved, on the other hand can be further increased
Toughness, bending strength and cracking resistance of product etc..Meanwhile by the way of three-stage sintering, control organic in ceramic powder
The content of solvent is 5-8wt%, and one-stage sintering removes organic solvent and the channel of nitrogen in basal body structure, is conducive to the nitrogen of silica flour
Change；Bis sintering makes silica flour fully nitrogenize and under the action of boron nitride nano-tube, silicon carbide whisker and sintering aid and α-
Silicon nitride is combined closely, while silica flour and α-siliconnitride occur to turn to the crystal form of beta-silicon nitride under beta-silicon nitride inducing action
Become, obtains the product that intensity is high, compactness is good；Three-stage sintering further strengthens product, makes the mechanical property and chemistry of product
Stability is further enhanced.
Silicon nitride ceramics provided by the invention is made by above-mentioned preparation method, therefore correspondingly has good toughness, bending resistance
The features such as intensity is high and cracking resistance is good.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Silicon nitride ceramics of the embodiment of the present invention and preparation method thereof is specifically described below.
The present invention provides a kind of preparation method of silicon nitride ceramics, including：
S1, raw material is uniformly mixed to get ceramic powder.
S2, ceramic powder is pressed into biscuit of ceramics.
S3, biscuit of ceramics is sintered to obtain silicon nitride ceramics.
In S1 steps, raw material includes：Silica flour, α-siliconnitride, beta-silicon nitride, boron nitride nano-tube, silicon carbide whisker, metal
Oxide and rare earth oxide.
Optionally, which counts in parts by weight includes：20-30 parts of silica flour, 100-120 parts of α-siliconnitride, beta-silicon nitride
2-5 parts of 4-6 parts, 5-8 parts of boron nitride nano-tube, 10-15 parts of silicon carbide whisker, 1-2 parts of metal oxide and rare earth oxide.
Still optionally further, which counts in parts by weight includes：25-30 parts of silica flour, 100-115 parts of α-siliconnitride, β-
5-6 parts of silicon nitride, 5-6 parts of boron nitride nano-tube, 12-15 parts of silicon carbide whisker, 1-2 parts of metal oxide and rare earth oxide
3-5 parts.
Further optionally, which counts in parts by weight includes：25 parts of silica flour, 115 parts of α-siliconnitride, beta-silicon nitride
3 parts of 5 parts, 6 parts of boron nitride nano-tube, 12 parts of silicon carbide whisker, 1 part of metal oxide and rare earth oxide.
The purity of silica flour is not less than 99%, and granularity is less than 74 μm.α-siliconnitride is that purity is about more than 99%, average grain diameter
0.5 μm of powder.Beta-silicon nitride is the crystal seed that diameter is about 0.5-1 μm, draw ratio is 7-10.
The present invention is sintered using silica flour and the compound system of α-siliconnitride and beta-silicon nitride, based on α-siliconnitride
Nitridation generates silicon nitride between wanting basis material, silica flour to be distributed evenly in α-siliconnitride, is conducive to improve silicon nitride ceramics
Consistency.
Wherein, α-siliconnitride can generate channel of nitrogen, improve the nitriding rate of silica flour, improve the structure of tissue.Beta-silicon nitride
Crystal transfer to beta-silicon nitride occurs for the silicon nitride that induction α-siliconnitride and silica flour generate and the surface in beta-silicon nitride is given birth to
Long, to increase product consistency and mechanical strength, the densification degree of obtained silicon nitride ceramics, intensity and toughness are higher.
On this basis, boron nitride nano-tube, silicon carbide whisker are introduced, the nitrogen that α-siliconnitride is generated with silica flour can be improved
Bonding strength between SiClx and tight ness rating.Meanwhile silicon carbide whisker is used to increase the toughness of silicon nitride ceramics, due to silicon carbide
Linear expansion coefficient can generate tangential residual stress in the base in sintering process, make external force right much larger than silicon nitride
When silicon nitride ceramics acts on, inherent residual stress is first offset, achievees the purpose that stress toughening.Further, since two kinds of materials
Expansion coefficient difference, micro-crack can be generated in the base, can equally play the role of offset external force, reach microcrack evolution equation
Purpose.Meanwhile silicon carbide whisker can be such that the crystal grain of ceramic material further refines, and ceramic material is made preferably to be densified, and carry
Its high mechanical strength.The interface cohesion of boron nitride nano-tube and silicon nitride ceramics is good, in cooperation silicon carbide whisker makes matrix
In the case of generating micro-crack, the stress of silicon nitride ceramics crack tip can be absorbed, effectively prevents in silicon nitride matrix and produces
Raw big stress concentration, when near crack propagation to silicon carbide whisker, crack tip can form strong stress shielding area, increase
The resistance of crack propagation is conducive to the intensity and cracking resistance that improve silicon nitride ceramics, makes the modifying function of silicon carbide whisker
Further controllableization.
Metal oxide and rare earth oxide promote crystal transfer of the α-siliconnitride to beta-silicon nitride as sintering aid,
The homogenizing for being conducive to material structure is conducive to the bending strength and fracture toughness that improve material.
Further, it is 1-2 that metal oxide, which includes mass ratio,:1 aluminium oxide and zirconium oxide.Be conducive to the entirety of crystal
Development.
Rare earth oxide includes that mass ratio is 1:The yttrium oxide and lanthana of 2-3.Can promote beta-silicon nitride formation and
Growth, while the draw ratio of beta-silicon nitride can be further increased, the addition of aluminium oxide and zirconium oxide is made up to beta-silicon nitride
It influences.The silicon nitride ceramics made has uniform microstructure, and bending strength and fracture toughness are good.
Raw material is mixed using organic solvent, and drying operation is carried out after the completion of mixing, and raw material is made to be uniformly mixed.
Specifically, the mixing of raw material and organic solvent is completed using ball milling operation, the rotating speed of ball milling be 400-800r/min,
Time is 2-3h.Ball milling operation can obtain raw material and form the slurries mixed well with organic solvent；Raw material is lived simultaneously
Change, raw material granularity is made to reach micro-nano, induces the faults of construction such as dislocation, vacancy, reactivity is made to enhance.
Drying operation carries out under conditions of 120-150 DEG C of temperature, removes most of organic solvent.Obtained ceramic powder
Body, the content for controlling its solvent are 5-8wt%.Organic solvent evaporation and the channel of nitrogen in basal body structure, are conducive in sintering
The nitridation of silica flour.The content of organic solvent needs stringent control in ceramic powder, and the content of organic solvent is too small, is unfavorable for silica flour
Abundant nitridation, influence the crystal structure of silicon nitride ceramics；The content of organic solvent is excessive, leads to the consistency of silicon nitride ceramics
It is affected.
In some optional embodiments of the invention, the quality summation of raw material and the mass ratio of organic solvent are 1:
1.5-2 is conducive to mixing well for each ingredient in abundant ball milling and raw material.
Further, organic solvent includes at least two in methanol, ethyl alcohol and acetone, if the organic solvent can be first
Alcohol and ethyl alcohol combination, methanol and acetone combination, ethyl alcohol and acetone combination or methanol, ethyl alcohol and third
The combination of ketone three.It is combined using at least two organic solvents, successively evaporation forms channel of nitrogen, the nitrogen of silica flour in sintering
Change fully, while being conducive to the homogenization of structure.
In S2 steps, the pressing operation of ceramic powder uses cold isostatic pressing method, briquetting pressure 180-250MPa.
Silicon nitride has smaller constriction coefficient, can be suppressed according to the size of final finished in cold isostatic compaction, then into
Row sintering.
In S3 steps, the sintering of biscuit of ceramics includes the one-stage sintering sequentially carried out, bis sintering and three sections of burnings
Tie three section operation.It specifically includes：
Biscuit of ceramics is subjected to one-stage sintering under the conditions of nitrogen pressure 0.1-0.3MPa, 200-300 DEG C of temperature；Then exist
Bis sintering is carried out under the conditions of nitrogen pressure 0.1-0.3Mpa, 1400-1500 DEG C of temperature；Finally nitrogen pressure 1.5-2Mpa,
Three-stage sintering is carried out under the conditions of 1700-1800 DEG C of temperature.
Optionally, the time of one-stage sintering is 1-2h, and the time of bis sintering is 3-5h, and the time of three-stage sintering is 6-
8h。
One-stage sintering carries out under in contrast compared with low pressure and lower temperature, and organic solvent contains in cooperation ceramic powder
Amount is the characteristic of 5-8wt%, main to remove organic solvent and the channel of nitrogen in basal body structure, is conducive to the nitridation of silica flour.
Bis sintering makes silica flour fully nitrogenize and under the action of boron nitride nano-tube, silicon carbide whisker and sintering aid
It combines closely with α-siliconnitride, while the crystal form to beta-silicon nitride occurs under beta-silicon nitride inducing action for silica flour and α-siliconnitride
Transformation obtains the product that intensity is high, compactness is good.
Three-stage sintering further strengthens product, and the mechanical property of product and chemical stability is made to be further enhanced.
It is to be made by the preparation method of above-mentioned silicon nitride ceramics, therefore the present invention also provides a kind of silicon nitride ceramics
Correspondingly also has the features such as good toughness, bending strength are high and cracking resistance is good.
Further, which is silicon nitride ceramics pin.Biscuit of ceramics is pressed into and nitrogen on demand when preparation
The corresponding shape size structure of SiClx ceramic pins, or sintered silicon nitride ceramics is processed finishing, obtain silicon nitride
Ceramic pins.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of silicon nitride ceramics, including：
S1, it is 25 parts of silica flour, 115 parts of α-siliconnitride, 5 parts of beta-silicon nitride, boron nitride nano-tube 6 in parts by weight
Part, 12 parts of silicon carbide whisker, 1 part of metal oxide and 3 parts of rare earth oxide are on the waiting list raw material.By raw material and organic solvent according to
Mass ratio is 1:1.5 mixing, use silicon nitride abrading-ball, the rotating speed ball milling 3h with 600r/min, then at 130 DEG C in the ball mill
Under be dried to organic solvent content be 6wt%, obtain ceramic powder.
Wherein：Metal oxide is that mass ratio is 1:1 aluminium oxide and zirconium oxide；Rare earth oxide is that mass ratio is 1:2
Yttrium oxide and lanthana；Organic solvent is that mass ratio is 1:1 absolute ethyl alcohol and acetone.
S2, ceramic powder is subjected to cold isostatic compaction compacting using the pressure of 220MPa, obtains biscuit of ceramics.
S3, biscuit of ceramics is subjected to one-stage sintering under the conditions of nitrogen pressure 0.2Mpa, 200-300 DEG C of temperature, the time is
1.5h；Then bis sintering, time 4h are carried out under the conditions of nitrogen pressure 0.3Mpa, 1400-1500 DEG C of temperature；Finally in nitrogen
Three-stage sintering, time 7h are carried out under the conditions of atmospheric pressure 1.8Mpa, 1700-1800 DEG C of temperature.Obtain silicon nitride ceramics.
Embodiment 2
A kind of preparation method of silicon nitride ceramics, including：
S1, it is 20 parts of silica flour, 120 parts of α-siliconnitride, 4 parts of beta-silicon nitride, boron nitride nano-tube 8 in parts by weight
Part, 10 parts of silicon carbide whisker, 2 parts of metal oxide and 2 parts of rare earth oxide are on the waiting list raw material.By raw material and organic solvent according to
Mass ratio is 1:2 mixing, use silicon nitride abrading-ball, the rotating speed ball milling 3h with 400r/min, then at 130 DEG C in the ball mill
It is 5wt% to be dried to organic solvent content, obtains ceramic powder.
Wherein：Metal oxide is that mass ratio is 2:1 aluminium oxide and zirconium oxide；Rare earth oxide is that mass ratio is 1:3
Yttrium oxide and lanthana；Organic solvent is that mass ratio is 1:1 methanol and acetone.
S2, ceramic powder is subjected to cold isostatic compaction compacting using the pressure of 220MPa, obtains biscuit of ceramics.
S3, biscuit of ceramics is subjected to one-stage sintering under the conditions of nitrogen pressure 0.1Mpa, 200-300 DEG C of temperature, the time is
2h；Then bis sintering, time 5h are carried out under the conditions of nitrogen pressure 0.1Mpa, 1400-1500 DEG C of temperature；Finally in nitrogen
Three-stage sintering, time 6h are carried out under the conditions of pressure 2Mpa, 1700-1800 DEG C of temperature.Obtain silicon nitride ceramics.
Embodiment 3
A kind of preparation method of silicon nitride ceramics, including：
S1, it is 30 parts of silica flour, 100 parts of α-siliconnitride, 6 parts of beta-silicon nitride, boron nitride nano-tube 5 in parts by weight
Part, 15 parts of silicon carbide whisker, 1 part of metal oxide and 5 parts of rare earth oxide are on the waiting list raw material.By raw material and organic solvent according to
Mass ratio is 1:1.8 mixing, use silicon nitride abrading-ball, the rotating speed ball milling 2h with 800r/min, then at 130 DEG C in the ball mill
Under be dried to organic solvent content be 8wt%, obtain ceramic powder.
Wherein：Metal oxide is that mass ratio is 2:1 aluminium oxide and zirconium oxide；Rare earth oxide is that mass ratio is 1:2
Yttrium oxide and lanthana；Organic solvent is that mass ratio is 1:1 methanol and absolute ethyl alcohol.
S2, ceramic powder is subjected to cold isostatic compaction compacting using the pressure of 220MPa, obtains biscuit of ceramics.
S3, biscuit of ceramics is subjected to one-stage sintering under the conditions of nitrogen pressure 0.3Mpa, 200-300 DEG C of temperature, the time is
1h；Then bis sintering, time 3h are carried out under the conditions of nitrogen pressure 0.3Mpa, 1400-1500 DEG C of temperature；Finally in nitrogen
Three-stage sintering, time 8h are carried out under the conditions of pressure 1.5Mpa, 1700-1800 DEG C of temperature.Obtain silicon nitride ceramics.
Embodiment 4
A kind of preparation method of silicon nitride ceramics, difference from example 1 is that：
Metal oxide is aluminium oxide, and rare earth oxide is yttrium oxide.
Embodiment 5
A kind of preparation method of silicon nitride ceramics, difference from example 1 is that：
Organic solvent is absolute ethyl alcohol.
Comparative example 1
A kind of preparation method of silicon nitride ceramics, difference from example 1 is that：
The content of organic solvent is no more than 1wt% in ceramic powder.
Comparative example 2
A kind of preparation method of silicon nitride ceramics, difference from example 1 is that：
Boron nitride nano-tube uses the replacement of the silicon carbide whisker of equal quality.
Test example
Silicon nitride ceramics made from embodiment 1-5 and comparative example 1-2 is tested for the property comprising：It is curved using 3 points
Bent method measures bending strength and fracture toughness, and density is measured by drainage, measures that the results are shown in Table 1.
1 silicon nitride ceramics performance test table of table
In conclusion the preparation method of silicon nitride ceramics provided by the invention, uses silica flour and α-siliconnitride and β-nitrogen
The compound system of SiClx is sintered, using α-siliconnitride as major matrix material, silica flour be distributed evenly in α-siliconnitride it
Between nitridation generate silicon nitride, be conducive to improve silicon nitride ceramics consistency；α-siliconnitride can generate channel of nitrogen, improve silica flour
Nitriding rate, improve the structure of tissue；The silicon nitride that beta-silicon nitride induces α-siliconnitride and silica flour to generate occurs to β-nitridation
The crystal transfer of silicon, to increase product consistency and mechanical strength.On this basis, boron nitride nano-tube, silicon carbide whisker are introduced
Must, it on the one hand can improve the bonding strength and tight ness rating between the silicon nitride that α-siliconnitride and silica flour generate, another aspect energy
Enough further increase the toughness, bending strength and cracking resistance etc. of product.Meanwhile by the way of three-stage sintering, control pottery
The content of organic solvent is 5-8wt% in porcelain powder, and one-stage sintering removes organic solvent and the channel of nitrogen in basal body structure, profit
In the nitridation of silica flour；Bis sintering makes silica flour fully nitrogenize and in boron nitride nano-tube, silicon carbide whisker and sintering aid
Effect is lower to combine closely with α-siliconnitride, while silica flour and α-siliconnitride occur under beta-silicon nitride inducing action to beta-silicon nitride
Crystal transfer, obtain the product that intensity is high, compactness is good；Three-stage sintering further strengthens product, makes the mechanical property of product
Energy and chemical stability are further enhanced.
Silicon nitride ceramics provided by the invention is made by above-mentioned preparation method, therefore correspondingly has good toughness, bending resistance
The features such as intensity is high and cracking resistance is good.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silicon nitride ceramics, which is characterized in that including：
Raw material is mixed and dried using organic solvent, ceramic powder is obtained, the raw material includes silica flour, α-siliconnitride, β-nitrogen
SiClx, boron nitride nano-tube, silicon carbide whisker, metal oxide and rare earth oxide, it is organic described in the ceramic powder
The content of solvent is 5-8wt%；
The ceramic powder is pressed into biscuit of ceramics；
The biscuit of ceramics is subjected to one-stage sintering under the conditions of nitrogen pressure 0.1-0.3MPa, 200-300 DEG C of temperature；Then exist
Bis sintering is carried out under the conditions of nitrogen pressure 0.1-0.3Mpa, 1400-1500 DEG C of temperature；Finally nitrogen pressure 1.5-2Mpa,
Three-stage sintering is carried out under the conditions of 1700-1800 DEG C of temperature.
2. preparation method according to claim 1, which is characterized in that the raw material is counted in parts by weight includes：The silicon
It is 20-30 parts of powder, α-siliconnitride 100-120 parts described, beta-silicon nitride 4-6 parts described, boron nitride nano-tube 5-8 parts described, described
It is 10-15 parts of silicon carbide whisker, metal oxide 1-2 parts and rare earth oxide 2-5 parts described described.
3. preparation method according to claim 1 or 2, which is characterized in that the mixing of the raw material and the organic solvent
It is completed using ball milling operation, the rotating speed of ball milling is 400-800r/min, time 2-3h.
4. preparation method according to claim 3, which is characterized in that the quality summation of the raw material and the organic solvent
Mass ratio be 1:1.5-2.
5. preparation method according to claim 3, which is characterized in that the organic solvent includes methanol, ethyl alcohol and acetone
In at least two.
6. preparation method according to claim 1 or 2, which is characterized in that the time of one-stage sintering is 1-2h, bis sintering
Time be 3-5h, time of three-stage sintering is 6-8h.
7. preparation method according to claim 6, which is characterized in that the metal oxide includes that mass ratio is 1-2:1
Aluminium oxide and zirconium oxide.
8. preparation method according to claim 6, which is characterized in that the rare earth oxide includes that mass ratio is 1:2-3
Yttrium oxide and lanthana.
9. the silicon nitride ceramics made from claim 1-8 any one of them preparation methods.
10. silicon nitride ceramics according to claim 9, which is characterized in that the silicon nitride ceramics is silicon nitride ceramics pin.
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