CN100372804C - Method of self propagating reaction sinterad Si3N4BN complex phase processable ceramic - Google Patents
Method of self propagating reaction sinterad Si3N4BN complex phase processable ceramic Download PDFInfo
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- CN100372804C CN100372804C CNB2006100890136A CN200610089013A CN100372804C CN 100372804 C CN100372804 C CN 100372804C CN B2006100890136 A CNB2006100890136 A CN B2006100890136A CN 200610089013 A CN200610089013 A CN 200610089013A CN 100372804 C CN100372804 C CN 100372804C
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Abstract
The present invention relates to a method capable of utilizing auto-spreading reaction sintering process to prepare Si3N4/BN double phase workable ceramics, belonging to the field of auto-spreading high-temperature synthesis technology. The buried powder adopted by chemical furnace is a mixed powder made up by mixing Si powder and Si3N4 powder, their mixing ratio is: Si powder content is 50-70 wt% and Si3N4 powder content is 30-50 wt%. Si3N4/BN workable ceramic raw material mixing ratio is as follows: BN powder content is 15-35 volume%, Si powder content is 65-85 volume%, besides adding 2-14 wt% of Al2O3 powder, N2 pressure of SHS reaction is 4-10MPa. The mixing ration of Si3N4/BN workable ceramic raw material in which Si3N4 powder diluting agent is added is as follows: BN powder content is 15-35 volume%, Si powder content is 40-60 volume%, Si3N4 powder diluting agent content is 5-45 volume%, besides adding 2-14 wt% of Al2O3 powder, N2 pressure of SHS reaction is 4-10 MPa.
Description
Technical field
The invention belongs to the self propagating high temperature synthesis technical field, a kind of self-propagating reaction sintering Si particularly is provided
3N
4The method of/BN complex phase processable ceramic.
Background technology
Since The former Russian scholar A.G.Merzhanov in 1967 and I.P.Borovinskaya found the SHS phenomenon, SHS was one of the research direction in Materials Science and Engineering field always.
Self propagating high temperature synthetic technology characteristics are: light reactant powders or powder compact, by high heat-producing chemical reaction takes place between the powder, feasible contiguous powder temperature raises and causes it new reaction takes place, thereby make reaction be spread to entire reaction material district, final synthetic materials with the form of combustion wave.
The self propagating high temperature synthetic technology has many advantages:
(1) the burning building-up process has made full use of the chemical energy of reactant, does not need supplementing energy generally speaking, and energy consumption is low.
(2) owing to the energy that has utilized reactant self to be contained, combustionvelocity is fast, and process is of short duration, thereby the production efficiency height.
(3) simultaneously because high thermograde is easy to obtain the active very high steady mutually product of Jie and the material with high concentration fault of construction with fast cooling velocity.
(4) to make most impurity be able to evaporated product purity very high for the temperature of reaction height.
(5) the burning building-up process does not need high-temperature heater, and equipment is simple, invests little.
Silicon nitride ceramics is with its excellent high temperature, high strength, and over-all properties such as anti-environmental activity, be expected to become engineering use in one of stupalith of most worthy.But silicon nitride ceramics is difficult to processing as most of structural ceramicss has limited its application.For improving its machinability, people have done many research work in recent years: 1. Wang Xiangdong etc. adopts chemical solution method, has synthesized with nano-scale h-BN to coat a micron Si
3N
4Composite granule, this composite granule goes out both to have higher force through hot pressing and learns performance, the complex phase ceramic that has again better machinability simultaneously.2. Kawai etc. is at preparation Si
3N
4During porous material, generate selectively column β-Si
3N
4, to form column β-Si
3N
4Crystal grain is connected into the porous ceramics of closed pore at random mutually at three-dimensional.The porous SiN ceramic that their discovery has above-mentioned microstructure is 38% o'clock in porosity, and flexural strength reaches 455MPa, and is easy to process with carbamide tool.3. Wang Rui has just waited the thought with functionally gradient (FGM) to be incorporated in the processable ceramic design, and having prepared central core is pure Si
3N
4The Si with symmetrical structure that the phase both sides increase progressively for h-BN content
3N
4/ h-BN complex phase ceramic.Whole ceramic block top layer has good machinability, simultaneously because the pure Si of heart section
3N
4Make ceramic block keep higher mechanical property.But this several method sintering temperature height, energy consumption is big, and because being subjected to the device-restrictive product size littler, has therefore hindered its production and practical application.
Summary of the invention
The object of the present invention is to provide a kind of self-propagating reaction sintering Si
3N
4The method of/BN complex phase processable ceramic.Realized that technology is simple, sintering velocity is fast, and energy consumption is low, the efficient height.
The present invention adopts the Si powder, and the h-BN powder is raw material, with Al
2O
3Powder is sinter additives, Si
3N
4Powder is diluent, by adjusting the raw material proportioning, after the material base moulding, imbeds SHS " chemical stove ", and igniting is carried out the self-propagating reaction sintering and prepared the large-sized Si of peacekeeping two dimension
3N
4/ BN complex phase processable ceramic.
(1) buried powder of " chemical stove " employing is Si powder and Si
3N
4The mixed powder of powder.Its proportioning is: Si powder content 50～70 weight %, Si
3N
4Powder content 30～50 weight %.
(2) for not adding Si
3N
4The Si of powder diluent
3N
4/ BN processable ceramic raw material proportioning is: the h-BN powder content is 15～35 volume %, and the Si powder content is 65～85 volume %, adds 2～14 weight %Al again
2O
3Powder, material base relative density 50～80%, the N of SHS reaction
2Pressure 4～10MPa.
(3) for adding Si
3N
4The Si of powder diluent
3N
4/ BN processable ceramic raw material proportioning is: the h-BN powder content is 15～35 volume %, and the Si powder content is 40～60 volume %, Si
3N
4Content 5～45 volume % of powder diluent add 2～14 weight %Al again
2O
3Powder, material base relative density 50～80%, the N of SHS reaction
2Pressure 4～10MPa.
Principle of the present invention and advantage are summarized as follows:
Utilize Si and N
2Synthetic Si
3N
4High and the volume increase of the adiabatic combustion temperature of reaction, and the good characteristics of h-BN pottery machinability, for improving the machinability of silicon nitride ceramic material, this method is to form weak interface with h-BN in silicon nitride ceramics.When adding man-hour, can form tiny crack on the weak interface, and deflect along weak interface, the energy of dissipation crack propagation stops crack propagation; When load continues to rise, will produce new critical crack at the weak bonding interface place of lower floor and expand again; So repeatedly, make crackle become the stepped expansion of great-jump-forward, fracture takes place gradually but not the moment brittle failure makes stupalith have workability.
Operational path: (1) raw material is crossed the sub-granulation of 100 mesh sieves (4) material base moulding (5) by 5 hours (3) dry good powders of specified proportion ingredient (2) batch mixing the material base that presses is imbedded in " chemical stove ", lights in autoclave then and carries out the self-propagating reaction sintering.
This method and other preparation methods (normal pressure-sintered, hot pressed sintering, reaction-sintered) its advantage of comparing is: raw material adopts the Si powder, than with Si
3N
4Powder is that cost of material is low; The needed energy of sintering is provided by raw material self heat release fully, does not need firing equipment and has greatly saved the energy; Technology is simple, and sintering velocity is fast, the efficient height; The product processability is good, is fit to the preparation one dimension, the large scale goods of two dimension.
Embodiment
Example 1: the Si that does not add diluent
3N
4/ BN processable ceramic
Test used Si powder purity 99.6%, granularity 1 μ m; H-BN powder purity 98%, granularity 200 orders.Reactant content: the Si powder is 67 volume %, and the h-BN powder is 33 volume %, adds the Al of 6 weight % again
2O
3Powder is as sintering aid.In nylon ball grinder, be medium with the dehydrated alcohol, batch mixing 5h is then at 80 ℃ of dry 15h.Claim the dry good material of 6.5g in punching block, to make the stripe shape material base that is of a size of 8 * 10 * 55mm, material base relative density about 50% with defeating of 12MPa.
In the graphite material boat, the material base that presses is embedded in 60 weight %Si powder+40 weight %Si
3N
4Mixing buried powder (Si powder and the Si of powder
3N
4Cross 100 purpose sieves after the powder hand is mixed) in.In the synthetic autoclave of 10 liters of horizontal self propagating high temperatures, be filled with nitrogen then, an end is made igniting agent with titanium valve, lights with tungsten filament, carries out self propagating high temperature and synthesizes.Nitrogen pressure 6.5MPa, striking voltage 110V, electric current 10A.
Example 2: the Si that adds diluent
3N
4/ BN processable ceramic is tested used Si powder purity 99.6%, granularity 1 μ m; H-BN powder purity 98%, granularity 200 orders; Si
3N
4Powder purity is greater than 95%, and granularity is less than 300 orders.Reactant content: the Si powder is 50 volume %, and the h-BN powder is 33 volume %, adds 17 volume %Si
3N
4Powder is diluent, adds the Al of 6 weight % again
2O
3Powder is as sintering aid.Other technologies are identical with example 1.
Claims (2)
1. self-propagating reaction sintering Si
3N
4The method of/BN complex phase processable ceramic is characterized in that: for not adding Si
3N
4The Si of powder diluent
3N
4/ BN processable ceramic raw material proportioning is: the h-BN powder content is 15～35 volume %, and the Si powder content is 65～85 volume %, adds 2～14 weight %Al again
2O
3Powder, material base relative density 50～80%, the buried powder that chemical stove adopts is Si powder and Si
3N
4The mixed powder of powder, its proportioning is: the Si powder content is 50～70 weight %, Si
3N
4Powder content is 30～50 weight %; The N of SHS reaction
2Pressure is 4～10MPa.
2. it is characterized in that in accordance with the method for claim 1: for adding Si
3N
4The Si of powder diluent
3N
4/ BN processable ceramic raw material proportioning is: the h-BN powder content is 15～35 volume %, and the Si powder content is 40～60 volume %, Si
3N
4Content 5～45 volume % of powder diluent add 2～14 weight %Al again
2O
3Powder, material base relative density 50～80%, the N of SHS reaction
2Pressure is 4～10MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100890136A CN100372804C (en) | 2006-07-28 | 2006-07-28 | Method of self propagating reaction sinterad Si3N4BN complex phase processable ceramic |
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|---|---|---|---|
| CNB2006100890136A CN100372804C (en) | 2006-07-28 | 2006-07-28 | Method of self propagating reaction sinterad Si3N4BN complex phase processable ceramic |
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|---|---|
| CN1903789A CN1903789A (en) | 2007-01-31 |
| CN100372804C true CN100372804C (en) | 2008-03-05 |
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| CN103086720A (en) * | 2013-01-25 | 2013-05-08 | 西安交通大学 | Rapid nitridation preparation method of silicon nitride-boron nitride composite ceramic though reactive sintering |
| CN114406258B (en) * | 2022-01-25 | 2024-04-30 | 华清平耐磨科技(苏州)有限公司 | Thermite reduction reaction powder coated ZTA ceramic particles and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1145344A (en) * | 1995-08-28 | 1997-03-19 | 大连理工大学 | Method of using self-spreading high temp synthesis for prepn. of foamed ceramic materials |
| CN1194959A (en) * | 1998-03-09 | 1998-10-07 | 冶金工业部钢铁研究总院 | Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis |
| CN1557709A (en) * | 2004-02-10 | 2004-12-29 | 中国科学院上海硅酸盐研究所 | Preparation method of self-spread high-temperature synthesizing silicon nitride magnesium powder |
-
2006
- 2006-07-28 CN CNB2006100890136A patent/CN100372804C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1145344A (en) * | 1995-08-28 | 1997-03-19 | 大连理工大学 | Method of using self-spreading high temp synthesis for prepn. of foamed ceramic materials |
| CN1194959A (en) * | 1998-03-09 | 1998-10-07 | 冶金工业部钢铁研究总院 | Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis |
| CN1557709A (en) * | 2004-02-10 | 2004-12-29 | 中国科学院上海硅酸盐研究所 | Preparation method of self-spread high-temperature synthesizing silicon nitride magnesium powder |
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