CN110105072A - A kind of preparation method of high hardness silicon nitride material - Google Patents
A kind of preparation method of high hardness silicon nitride material Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of high hardness silicon nitride material, comprising the following steps: S1, mixing: each and binder and solvent of high hardness silicon nitride material are stirred 0.1-24h in blender to be uniformly mixed；S2, it is evaporated: mixture being evaporated to obtain solid powder；S3, molding: powder is obtained to the blocks of solid of certain shapes by the method for compression moulding or extrusion molding or injection molding；S4, degreasing: being heat-treated in debinding furnace by heat treatment method, removes the binder in solid；S5, sintering: the solid after degreasing is sintered in sintering furnace, obtains fine and close product.Modifying agent can increase the hardness of material in raw material, and related auxiliaries is combined to accelerate the compactness of product during the sintering process, and by addition silicon carbide, have adjusted the toughness of product, to obtain hardness height, the high product of intensity.
Description
Technical field
The present invention relates to silicon nitride material production fields, and in particular to a kind of preparation method of high hardness silicon nitride material.
Background technique
Silicon nitride is a kind of important structural ceramic material.It is a kind of superhard substance, itself has lubricity, and
It is wear-resistant, it is atomic crystal；It is anti-oxidant when high temperature.And it can also resist cooling thermal impact, be heated in air 1000 DEG C with
On, quick refrigeration sharply heats again, will not fragmentation.There is so excellent characteristic, Ren Menchang just because of silicon nitride ceramics
Often it is utilized to the mechanical components such as manufacture bearing, blade of gas turbine, mechanical seal ring, permanent mold.If using high temperature resistant
And the silicon nitride ceramics not readily conducted heat manufactures the heating surfaces of engine components, diesel engine quality not only can be improved, saves
Fuel, and can be improved the thermal efficiency.China and the U.S., Japan and other countries all have developed this diesel engine.
Currently used silicon nitride sintering processing has HIP sintering, reaction-sintered, normal pressure-sintered, atmosphere pressures to burn
Knot.Wherein HIP sintering pressure is high, and the device is complicated, and manufacturing technique requirent is tight, and production efficiency is lower, at high cost.Reaction is burnt
The silicon nitride ceramics compactness for tying production is poor, and the porosity is high, and the unreacted reactant of remaining is finally had in product.It is normal pressure-sintered at
This is low, the product of sinterable various complicated shapes, high-efficient, from practical, silicon nitride it is normal pressure-sintered be research master
Want one of direction.Normal pressure-sintered general use liquid-phase sintering mode generally adds to prepare the silicon nitride ceramics of high compactness
Add sintering aid, make its at high temperature with the SiO of silicon nitride surface2Reaction forms liquid phase, heavy by the rearrangement of particle, dissolution-
The densification of shallow lake acceleration of sintering.But the prior art production silicon nitride material because its addition other modifications or help burn material sheet
The limited capacity of body causes the comprehensive performance of material to fail the desirable level for reaching silicon nitride material.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of high hardness silicon nitride material, and modifying agent is added and increases material
The hardness and strength of material, and related auxiliaries is combined to promote the compactness of product during the sintering process, so that it is high, strong to obtain hardness
Spend high product.
To achieve the above object, the present invention is achieved by following scheme:
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with binder and solvent stirring 0.1-24h for raw material powder to be uniformly mixed in blender, described
Raw material powder is raw material powder A or raw material powder B；
Raw material powder A is made of α-siliconnitride, boron nitride, aluminium oxide, calcium oxide and silicon carbide, wherein the matter of each component
Measure percentage are as follows: α-siliconnitride 80%-95%, boron nitride 1-15%, aluminium oxide 0.5-8%, calcium oxide 0.2-4.8%, carbonization
Silicon 0.1-10%；
Raw material powder B is made of α-siliconnitride, titanium nitride, yttrium oxide, calcium oxide and silicon carbide, wherein the matter of each component
Measure percentage are as follows: α-siliconnitride 80%-95%, titanium nitride 1-10%, yttrium oxide 0.1-2%, calcium oxide 0.1-5.5%, carbonization
Silicon 0.1-10%；
S2, it is evaporated: mixture being evaporated to obtain solid powder；
S3, molding: powder is obtained into certain shapes by the method for compression moulding or extrusion molding or injection molding
Blocks of solid；
S4, degreasing: blocks of solid obtained in step S3 is being not less than 600 in debinding furnace by heat treatment method
It is heat-treated at a temperature of DEG C, removes the binder in solid；
S5, sintering: the solid after step S4 degreasing is sintered in sintering furnace, sintering temperature 1600-2000
DEG C, sintering time 0.1-10h obtains high hardness silicon nitride material.
Preferably, one or more of binder CMC, PVA, PVB or waterglass, the additive amount of binder are original
Expect the 2-5% of powder quality.
Preferably, solvent is one or both of dehydrated alcohol, ionized water, it is further preferred that solvent is deionization
Water, additional amount are 0.5-1 times of raw material powder quality.
Preferably, solvent is deionized water in step S1, and the water content that rear solid powder is evaporated in step S2 is 4-6%.
Preferably, when raw material powder is raw material powder A, preheating temperature is 680 DEG C in step S4, is sintered temperature in step S5
Degree is 1700 DEG C, sintering time 2h.
Preferably, when raw material powder is raw material powder B, preheating temperature is 700 DEG C in step S4, is sintered temperature in step S5
Degree is 1750 DEG C, sintering time 1.8h.
The beneficial effects of the present invention are:
One, high hardness silicon nitride material is prepared using raw material powder A, addition boron nitride is conducive to improve sintered nitrogen
The hardness of silicon nitride material, because boron nitride hardness itself is very high, after boron nitride or titanium oxide is added under normal circumstances, after sintering
Product be difficult densification, have many holes, product is frangible.Therefore, the present invention is added to aluminium oxide again and two kinds of calcium oxide are helped
Agent can accelerate the compactness of product during the sintering process, and by addition silicon carbide, the toughness of product be had adjusted, to obtain
It is high to obtain hardness, the high product of intensity.
Two, high hardness silicon nitride material is prepared using raw material powder B, addition titanium nitride is conducive to improve sintered nitrogen
The hardness of silicon nitride material expands its range of work, and yttrium oxide and calcium oxide is added, silicon nitride material can be improved
Consistency, durability is higher, adds silicon carbide, adjusts the toughness of product, and processed and applied range is wider, by adjusting various add
Add the adding proportion of object, product densified sintering product at a lower temperature can be made, saves sintering cost.
To sum up tell, it is each in raw material powder A or raw material powder B in the preparation method of high hardness silicon nitride material of the present invention
Component cooperation, silicon nitride material obtained have the characteristics that hardness is high, compactness is high, good toughness, and each component ratio is in raw material
The optimal selection of many experiments arrived, if a kind of ratio of raw material is too high or too low, will lead to product consistency it is relatively low or
The decline of hardness, intensity.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, all other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with PVA and deionized water stirring 0.5h for raw material powder to be uniformly mixed in blender, raw material powder
The mass percent of each component in end are as follows: α-siliconnitride 80%, boron nitride 10%, aluminium oxide 2%, calcium oxide 3%, silicon carbide
The additive amount of 5%, PVA are the 3% of raw material powder quality；
S2, be evaporated: it is 4% that mixture, which is evaporated to moisture content, obtains solid powder；
S3, molding: powder is obtained to the blocks of solid of certain shapes by briquetting process；
S4, degreasing: being heat-treated in debinding furnace by heat treatment method, and treatment temperature is 680 DEG C, removes solid
In PVA；
S5, sintering: the solid after degreasing is sintered in sintering furnace, and 1700 DEG C of sintering temperature, sintering time 2h is obtained
Obtain high hardness silicon nitride material.
Embodiment 2:
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with PVA and deionized water stirring 0.5h for raw material powder to be uniformly mixed in blender, raw material powder
The mass percent of each component in end are as follows: α-siliconnitride 90%, boron nitride 5%, aluminium oxide 2%, calcium oxide 1%, silicon carbide
The additive amount of 2%, PVA are the 3% of raw material powder quality；
S2, be evaporated: it is 4% that mixture, which is evaporated to moisture content, obtains solid powder；
S3, molding: powder is obtained to the blocks of solid of certain shapes by briquetting process；
S4, degreasing: being heat-treated in debinding furnace by heat treatment method, and treatment temperature is 680 DEG C, removes solid
In PVA；
S5, sintering: the solid after degreasing is sintered in sintering furnace, and 1700 DEG C of sintering temperature, sintering time 2h is obtained
Obtain fine and close product.
Embodiment 3:
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with PVA and deionized water stirring 0.5h for raw material powder to be uniformly mixed in blender, raw material powder
The mass percent of each component in end are as follows: α-siliconnitride 85%, boron nitride 5%, aluminium oxide 2%, calcium oxide 1%, silicon carbide
The additive amount of 7%, PVA are the 3% of raw material powder quality；
S2, be evaporated: it is 4% that mixture, which is evaporated to moisture content, obtains solid powder；
S3, molding: powder is obtained to the blocks of solid of certain shapes by briquetting process；
S4, degreasing: being heat-treated in debinding furnace by heat treatment method, and treatment temperature is 680 DEG C, removes solid
In PVA；
S5, sintering: the solid after degreasing is sintered in sintering furnace, and 1700 DEG C of sintering temperature, sintering time 2h is obtained
Obtain fine and close product.
Embodiment 4:
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with PVA and deionized water stirring 0.5h for raw material powder to be uniformly mixed in blender, raw material powder
The mass percent of each component in end are as follows: α-siliconnitride 80%, titanium nitride 10%, yttrium oxide 2%, calcium oxide 3%, silicon carbide
The additive amount of 5%, PVA are the 3% of raw material powder quality；
S2, be evaporated: it is 4% that mixture, which is evaporated to moisture content, obtains solid powder；
S3, molding: powder is obtained to the blocks of solid of certain shapes by the method for compression moulding；
S4, degreasing: being heat-treated in debinding furnace by heat treatment method, and treatment temperature is 700 DEG C, removes solid
In binder；
S5, sintering: the solid after degreasing is sintered in sintering furnace, and 1750 DEG C of sintering temperature, sintering time 1.8h,
Obtain fine and close product.
Embodiment 5:
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with PVA and deionized water stirring 0.5h for raw material powder to be uniformly mixed in blender, raw material powder
The mass percent of each component in end are as follows: α-siliconnitride 90%, titanium nitride 5%, yttrium oxide 1%, calcium oxide 2%, silicon carbide
The additive amount of 2%, PVA are the 3% of raw material powder quality；
S2, be evaporated: it is 4% that mixture, which is evaporated to moisture content, obtains solid powder；
S3, molding: powder is obtained to the blocks of solid of certain shapes by the method for compression moulding；
S4, degreasing: being heat-treated in debinding furnace by heat treatment method, and treatment temperature is 700 DEG C, removes solid
In binder；
S5, sintering: the solid after degreasing is sintered in sintering furnace, and 1750 DEG C of sintering temperature, sintering time 1.8h,
Obtain fine and close product.
Embodiment 6
A kind of preparation method of high hardness silicon nitride material, comprising the following steps:
S1, mixing: with PVA and deionized water stirring 0.5h for raw material powder to be uniformly mixed in blender, raw material powder
The mass percent of each component in end are as follows: α-siliconnitride 85%, titanium nitride 5%, yttrium oxide 2%, calcium oxide 1%, silicon carbide
The additive amount of 7%, PVA are the 3% of raw material powder quality；
Silicon nitride material obtained by embodiment 1-6 is processed respectively with diamond tool, with the nitrogen of each embodiment
More 3mm × 4mm × 45mm battens are respectively prepared in silicon nitride material.The batten made of the silicon nitride material of embodiment 1 is denoted as
No. 1 batten, the batten made of the silicon nitride material of embodiment 2-6 are correspondingly denoted as 2-6 batten.1-6 batten is for surveying
Try the performance of silicon nitride material.
The silicon nitride material (1-6 batten) of embodiment 1-6 preparation performs the following performance tests:
(1) fracture toughness test: 6 are tested fracture toughness, three-point bending resistance with unilateral bridge notch method, and span 40mm is cut
Mouth is having a size of 150 ± 2um；
(2) bending strength test: 10 in every number batten are used to test the bending strength of silicon nitride, according to ASTM-
C1161-02 standard, 4 bending resistances, outer span 40mm, interior span 20mm；
(3) hardness test: 5kg Vickers is made a call to 30 points and is averaged；
Testing result is as shown in table 1 below.
Table 1:
As can be seen from Table 1, between 17-22.5Gpa, bending strength exists silicon nitride material hardness prepared by the present invention
Between 700-1050Mpa, hence it is evident that be higher than existing silicon nitride material.Therefore, the present invention be added boron nitride, titanium nitride, aluminium oxide and
The modified materials such as yttrium oxide obtain hardness height, the high product of intensity.Several additives ratios in the present invention need to cooperate,
Otherwise required actual effect cannot be taken into account or be obtained to performance, if the improper effect that will not have been obtained of ratio, this
Ratio is the preferred proportion obtained by many experiments.
In the description of this specification, the description meaning of reference term " one embodiment ", " example ", " specific example " etc.
Refer to that specific features described in conjunction with this embodiment or example, structure, material live feature and be contained at least one reality of the invention
It applies in example or example.In the present specification, schematic expression of the above terms are not necessarily referring to identical embodiment or show
Example.Moreover, particular features, structures, materials, or characteristics described can be in any one or more embodiment or examples
In can be combined in any suitable manner.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described to the greatest extent, also do not limit the specific embodiment that the invention is only.It obviously, can according to the content of this specification
It makes many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (6)
1. a kind of preparation method of high hardness silicon nitride material, which comprises the following steps:
S1, mixing: with binder and solvent stirring 0.1-24h for raw material powder to be uniformly mixed in blender, the raw material
Powder is raw material powder A or raw material powder B；
Raw material powder A is made of α-siliconnitride, boron nitride, aluminium oxide, calcium oxide and silicon carbide, wherein the quality percentage of each component
Than are as follows: α-siliconnitride 80%-95%, boron nitride 1-15%, aluminium oxide 0.5-8%, calcium oxide 0.2-4.8%, silicon carbide 0.1-
10%；
Raw material powder B is made of α-siliconnitride, titanium nitride, yttrium oxide, calcium oxide and silicon carbide, wherein the quality percentage of each component
Than are as follows: α-siliconnitride 80%-95%, titanium nitride 1-10%, yttrium oxide 0.1-2%, calcium oxide 0.1-5.5%, silicon carbide 0.1-
10%；
S2, it is evaporated: mixture being evaporated to obtain solid powder；
S3, molding: powder is obtained to the bulk of certain shapes by the method for compression moulding or extrusion molding or injection molding
Solid；
S4, degreasing: blocks of solid obtained in step S3 is being not less than in debinding furnace by 600 DEG C of temperature by heat treatment method
It is heat-treated under degree, removes the binder in solid；
S5, sintering: the solid after step S4 degreasing is sintered in sintering furnace, and sintering temperature is 1600-2000 DEG C, sintering
Time is 0.1-10h to get the high hardness silicon nitride material.
2. a kind of preparation method of high hardness silicon nitride material according to claim 1, it is characterised in that: the binder
For one or more of CMC, PVA, PVB, waterglass, the additive amount of binder is the 2-5% of raw material powder quality.
3. a kind of preparation method of high hardness silicon nitride material according to claim 1, it is characterised in that: the solvent is
One or both of dehydrated alcohol, ionized water.
4. a kind of preparation method of high hardness silicon nitride material according to claim 3, it is characterised in that: molten in step S1
Agent is deionized water, and the water content that rear solid powder is evaporated in step S2 is 4-6%.
5. a kind of preparation method of high hardness silicon nitride material according to claim 1, it is characterised in that: raw material powder is
When raw material powder A, preheating temperature is 680 DEG C in step S4, and sintering temperature is 1700 DEG C in step S5, sintering time 2h.
6. a kind of preparation method of high hardness silicon nitride material according to claim 1, it is characterised in that: raw material powder is
When raw material powder B, preheating temperature is 700 DEG C in step S4, and sintering temperature is 1750 DEG C in step S5, sintering time 1.8h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111499392A (en) * | 2020-04-24 | 2020-08-07 | 潍坊工商职业学院 | High-hardness ceramic and preparation method thereof |
| CN116477957A (en) * | 2023-05-05 | 2023-07-25 | 湖南泰鑫瓷业有限公司 | Heat-resistant ceramic cutter and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0175041A1 (en) * | 1984-09-19 | 1986-03-26 | Battelle Memorial Institute | Silicon nitride sintered bodies and a method for their production |
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| CN111499392A (en) * | 2020-04-24 | 2020-08-07 | 潍坊工商职业学院 | High-hardness ceramic and preparation method thereof |
| CN116477957A (en) * | 2023-05-05 | 2023-07-25 | 湖南泰鑫瓷业有限公司 | Heat-resistant ceramic cutter and preparation method and application thereof |
| CN116477957B (en) * | 2023-05-05 | 2024-03-12 | 湖南泰鑫瓷业有限公司 | Heat-resistant ceramic cutter and preparation method and application thereof |
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