CN110183233A - A kind of novel Si3N4Enhance MoSi2Based composites and preparation method - Google Patents

A kind of novel Si3N4Enhance MoSi2Based composites and preparation method Download PDF

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CN110183233A
CN110183233A CN201910504812.2A CN201910504812A CN110183233A CN 110183233 A CN110183233 A CN 110183233A CN 201910504812 A CN201910504812 A CN 201910504812A CN 110183233 A CN110183233 A CN 110183233A
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万细凤
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Abstract

The present invention relates to MoSi2Based composites technical field, and disclose a kind of novel Si3N4Enhance MoSi2Based composites and preparation method, the raw material including following parts by weight proportion: 20~30 parts of nano Si3N4Powder, 2~5 parts of gamma-aminopropyl-triethoxy-silane coupling agent, 5~8 parts of ball shaped nano Cu particle, 8~10 parts of polyvinyl alcohol, 60~70 parts of micron order MoSi2Powder.The present invention solves the Si prepared at present3N4Enhance MoSi2Based composites, the technical issues of all showing brittleness over the entire temperature range.

Description

A kind of novel Si3N4Enhance MoSi2Based composites and preparation method
Technical field
The present invention relates to MoSi2Based composites technical field, specially a kind of novel Si3N4Enhance MoSi2Base composite wood Material and preparation method.
Background technique
Certain structure members in modern aerospace system require material, can safe and reliable work at high temperature, There is lower dead load again, therefore the big high-temperature structural material of unit mass thrust increasingly causes to pay close attention to.And two silication Molybdenum (MoSi2) be a kind of intermetallic compound of high-melting-point (2030 DEG C) and good integrate the new of function and structure Profile material, and molybdenum disilicide (MoSi2) not only there is moderate density (16.24g/cm3), good thermal conductivity is (at 1100 DEG C For 28.5W/mk), can also 1200 DEG C or more at a temperature of work.
However, the biggest obstacle of limitation molybdenum disilicide application has following three aspects at present: (1) elevated temperature strength is low；(2) in Warm (200~800 DEG C) oxidation rate is fast；(3) black brittleness is big.It, can be in two silicon in order to improve the performance of molybdenum disilicide material Change and reinforced phase is added in Mo substrate, progress two-phase is compound, and MoSi is prepared2Based composites.And Si3N4Ceramic pole high temperature resistant, Intensity can maintain always the high temperature to 1200 DEG C not to be melt into melt body after heated without declining, until 1900 DEG C can just divide Solution, and have surprising resistance to chemical corrosion, and Si3N4Theoretical density be 3.1g/cm3Left and right, so Si3N4Ceramics can be used To enhance MoSi2Matrix.
But due to MoSi2With Si3N4Ability without alloying but also is prepared so not only processing relatively difficult Si3N4Ceramics enhancing MoSi2Based composites all show brittleness over the entire temperature range, therefore, using Si3N4Ceramics increase Strong MoSi2Based composites are used as structural material, still have very big risk.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of novel Si3N4Enhance MoSi2Based composites and preparation Method solves the Si prepared at present3N4Enhance MoSi2Based composites all show brittle over the entire temperature range Technical problem.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of novel Si3N4Enhance MoSi2Based composites, the raw material including following parts by weight proportion: 20~30 parts Nano Si3N4Powder, 2~5 parts of gamma-aminopropyl-triethoxy-silane coupling agent, 5~8 parts of ball shaped nano Cu particle, 8~10 Part polyvinyl alcohol, 60~70 parts of micron order MoSi2Powder.
Preferably, the average grain diameter of the ball shaped nano Cu particle is within the scope of 40~50nm.
Preferably, the MoSi2The average grain diameter of powder is 1.3um, the nano Si3N4The average grain diameter of powder is 100nm。
A kind of novel Si3N4Enhance MoSi2The preparation method of based composites, comprising the following steps:
(1) 20~30 parts of nano Si is weighed3N4Powder is placed in ball grinder together with 50 parts of dehydrated alcohols, is protected in nitrogen Shield is lower to carry out 1~3h of ball milling, later, 2~5 parts of gamma-aminopropyl-triethoxy-silane coupling agent is added, continues 2~4h of ball milling, Using the mixed solvent being made of in equal volume deionized water and dehydrated alcohol to the nano Si for wrapping up in slurry3N4Powder wash for 3~6 times It washs；
(2) by the above-mentioned nano Si for wrapping up in slurry3N4Powder is added in the reactor equipped with magnetic stirring apparatus, and to reactor The mixed solvent that middle addition 200mL is made of in equal volume deionized water and dehydrated alcohol, in the magnetic force that revolving speed is 120~180rpm Under stirring, 5~8 parts of ball shaped nano Cu particle is added in reactor, 1~3h of magnetic agitation under 300~500rpm is switched to, it Afterwards, centrifugal treating is carried out, the nano Si that surface uniform load has nano Cu particle is prepared3N4Powder；
(3) 8~10 parts of polyvinyl alcohol (PVA) are dissolved in the deionized water that 20 parts of temperature are 100 DEG C, are stirred to complete Dissolution, preparation obtain polyvinyl alcohol (PVA) adhesive；
(4) mixed solvent being made of 600mL deionized water and 400mL dehydrated alcohol is added to and is filled equipped with high-speed stirred It sets in the reactor with heating device, in the case where revolving speed is 500~800rpm stirring, first by the polyvinyl alcohol (PVA) of above-mentioned preparation Adhesive is added in reactor, then slowly by the micron order MoSi of 60~70g2Powder is added in reactor, finally will be upper The surface uniform load for stating preparation has the nano Si of nano Cu particle3N4Powder is added in reactor, and later, switching to temperature is 100~120 DEG C, rate be 800~1000rpm under react 2~4h, obtain being distributed uniform mixed slurry；
(5) the uniform mixed slurry of above-mentioned distribution is fitted into etc. in static pressure rubber mold, is suppressed under 65~80MPa pressure Molding, then be placed in preheating temperature and be in 600~800 DEG C of vacuum drying oven, with the heating rate of 5 DEG C/min, it is warming up to 1850~ 1900 DEG C, and 4h is kept the temperature under 1850~1900 DEG C, 10MPa, later with the annealing rate of 5 DEG C/min, taken when being cooled to room temperature Out, novel Si is prepared3N4Enhance MoSi2Based composites.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
The present invention is first in the Si of average grain diameter 100nm3N4Powder surface size, again load average partial size are in 40~50nm model Interior ball shaped nano Cu particle is enclosed, with average grain diameter is 1.3um's under the action of polyvinyl alcohol (PVA) adhesive later MoSi2Powder progress is compound, handles by hydrostatic profile, vacuum-sintering etc., novel Si is prepared3N4Enhance MoSi2Base is compound Material；Wherein, nanoscale Si3N4Powder and the MoSi close to nanosized2Powder after compound, is shown very excellent Flexility and plastic property, to solve Si3N4Enhance MoSi2Based composites all show over the entire temperature range The technical issues of brittleness.
Specific embodiment
Raw material used in the following embodiment is as follows:
Average grain diameter is the MoSi of 1.3um2Powder；
Average grain diameter is the Si of 100nm3N4Powder；
Ball shaped nano Cu particle of the average grain diameter within the scope of 40~50nm.
Embodiment one:
(1) Si that 20g average grain diameter is 100nm is weighed3N4Powder is placed in ball grinder together with 50g dehydrated alcohol, in nitrogen Ball milling 1h is carried out under gas shielded, later, 2g gamma-aminopropyl-triethoxy-silane coupling agent is added, is continued ball milling 2h, using by going The mixed solvent that ionized water and dehydrated alcohol form in equal volume is to the nano Si for wrapping up in slurry3N4Powder carries out 3 washings；
(2) by the above-mentioned nano Si for wrapping up in slurry3N4Powder is added in the reactor equipped with magnetic stirring apparatus, and to reactor The mixed solvent that middle addition 200mL is made of in equal volume deionized water and dehydrated alcohol, in the magnetic agitation that revolving speed is 120rpm Under, ball shaped nano Cu particle of the 5g average grain diameter within the scope of 40~50nm is added in reactor, magnetic force under 300rpm is switched to 1h is stirred, later, centrifugal treating is carried out, the nano Si that surface uniform load has nano Cu particle is prepared3N4Powder；
(3) 8g polyvinyl alcohol (PVA) is dissolved in 20mL temperature is in 100 DEG C of deionized water, stirring to being completely dissolved, Preparation obtains polyvinyl alcohol (PVA) adhesive；
(4) mixed solvent being made of 600mL deionized water and 400mL dehydrated alcohol is added to and is filled equipped with high-speed stirred It sets in the reactor with heating device, in the case where revolving speed is 500rpm stirring, first by polyvinyl alcohol (PVA) adhesive of above-mentioned preparation It is added in reactor, then the MoSi for being slowly 1.3um by the average grain diameter of 60g2Powder is added in reactor, finally will be upper The surface uniform load for stating preparation has the nano Si of nano Cu particle3N4Powder is added in reactor, and later, switching to temperature is 100 DEG C, rate be 800rpm under react 2h, obtain being distributed uniform mixed slurry；
(5) the uniform mixed slurry of above-mentioned distribution is fitted into etc. in static pressure rubber mold, is pressed under 65MPa pressure Type, then be placed in the vacuum drying oven that preheating temperature is 600 DEG C, with the heating rate of 5 DEG C/min, 1850 DEG C are warming up to, and in 1850 DEG C, keep the temperature 4h under 10MPa, later with the annealing rate of 5 DEG C/min, novel Si is prepared in taking-up when being cooled to room temperature3N4Increase Strong MoSi2Based composites；
(6) to the novel Si of above-mentioned preparation3N4Enhance MoSi2Based composites are tested for the property, and thermal conductivity is 83.1W/mk, density 9.2g/cm3。
Embodiment two:
(1) Si that 30g average grain diameter is 100nm is weighed3N4Powder is placed in ball grinder together with 50g dehydrated alcohol, in nitrogen Ball milling 3h is carried out under gas shielded, later, 5g gamma-aminopropyl-triethoxy-silane coupling agent is added, is continued ball milling 4h, using by going The mixed solvent that ionized water and dehydrated alcohol form in equal volume is to the nano Si for wrapping up in slurry3N4Powder carries out 6 washings；
(2) by the above-mentioned nano Si for wrapping up in slurry3N4Powder is added in the reactor equipped with magnetic stirring apparatus, and to reactor The mixed solvent that middle addition 200mL is made of in equal volume deionized water and dehydrated alcohol, in the magnetic agitation that revolving speed is 180rpm Under, ball shaped nano Cu particle of the 8g average grain diameter within the scope of 40~50nm is added in reactor, magnetic force under 500rpm is switched to 3h is stirred, later, centrifugal treating is carried out, the nano Si that surface uniform load has nano Cu particle is prepared3N4Powder；
(3) 10g polyvinyl alcohol (PVA) is dissolved in the deionized water that 20mL temperature is 100 DEG C, is stirred to completely molten Solution, preparation obtain polyvinyl alcohol (PVA) adhesive；
(4) mixed solvent being made of 600mL deionized water and 400mL dehydrated alcohol is added to and is filled equipped with high-speed stirred It sets in the reactor with heating device, in the case where revolving speed is 800rpm stirring, first by polyvinyl alcohol (PVA) adhesive of above-mentioned preparation It is added in reactor, then the MoSi for being slowly 1.3um by the average grain diameter of 70g2Powder is added in reactor, finally will be upper The surface uniform load for stating preparation has the nano Si of nano Cu particle3N4Powder is added in reactor, and later, switching to temperature is 120 DEG C, rate be 1000rpm under react 4h, obtain being distributed uniform mixed slurry；
(5) the uniform mixed slurry of above-mentioned distribution is fitted into etc. in static pressure rubber mold, is suppressed under 65~80MPa pressure Molding, then be placed in preheating temperature and be in 800 DEG C of vacuum drying oven is warming up to 1900 DEG C with the heating rate of 5 DEG C/min, and in 1900 DEG C, keep the temperature 4h under 10MPa, later with the annealing rate of 5 DEG C/min, taking-up when being cooled to room temperature is prepared novel Si3N4Enhance MoSi2Based composites；
(6) to the novel Si of above-mentioned preparation3N4Enhance MoSi2Based composites are tested for the property, and thermal conductivity is 86.1W/mk, density 9.2g/cm3。
Embodiment three:
(1) Si that 25g average grain diameter is 100nm is weighed3N4Powder is placed in ball grinder together with 50g dehydrated alcohol, in nitrogen Ball milling 2h is carried out under gas shielded, later, 4g gamma-aminopropyl-triethoxy-silane coupling agent is added, is continued ball milling 3h, using by going The mixed solvent that ionized water and dehydrated alcohol form in equal volume is to the nano Si for wrapping up in slurry3N4Powder carries out 5 washings；
(2) by the above-mentioned nano Si for wrapping up in slurry3N4Powder is added in the reactor equipped with magnetic stirring apparatus, and to reactor The mixed solvent that middle addition 200mL is made of in equal volume deionized water and dehydrated alcohol, in the magnetic agitation that revolving speed is 150rpm Under, ball shaped nano Cu particle of the 6g average grain diameter within the scope of 40~50nm is added in reactor, magnetic force under 400rpm is switched to 2h is stirred, later, centrifugal treating is carried out, the nano Si that surface uniform load has nano Cu particle is prepared3N4Powder；
(3) 9g polyvinyl alcohol (PVA) is dissolved in 20mL temperature is in 100 DEG C of deionized water, stirring to being completely dissolved, Preparation obtains polyvinyl alcohol (PVA) adhesive；
(4) mixed solvent being made of 600mL deionized water and 400mL dehydrated alcohol is added to and is filled equipped with high-speed stirred It sets in the reactor with heating device, in the case where revolving speed is 600rpm stirring, first by polyvinyl alcohol (PVA) adhesive of above-mentioned preparation It is added in reactor, then the MoSi for being slowly 1.3um by the average grain diameter of 65g2Powder is added in reactor, finally will be upper The surface uniform load for stating preparation has the nano Si of nano Cu particle3N4Powder is added in reactor, and later, switching to temperature is 110 DEG C, rate be 900rpm under react 3h, obtain being distributed uniform mixed slurry；
(5) the uniform mixed slurry of above-mentioned distribution is fitted into etc. in static pressure rubber mold, is suppressed under 65~80MPa pressure Molding, then be placed in preheating temperature and be in 600~800 DEG C of vacuum drying oven is warming up to 1900 DEG C with the heating rate of 5 DEG C/min, and 4h is kept the temperature under 1900 DEG C, 10MPa, later with the annealing rate of 5 DEG C/min, taking-up when being cooled to room temperature is prepared novel Si3N4Enhance MoSi2Based composites；
(6) to the novel Si of above-mentioned preparation3N4Enhance MoSi2Based composites are tested for the property, and thermal conductivity is 87.4W/mk, density 9.4g/cm3。

Claims (4)

1. a kind of novel Si3N4Enhance MoSi2Based composites, which is characterized in that the raw material including following parts by weight proportion: 20~30 parts of nano Si3N4Powder, 2~5 parts of gamma-aminopropyl-triethoxy-silane coupling agent, 5~8 parts of ball shaped nano Cu Particle, 8~10 parts of polyvinyl alcohol, 60~70 parts of micron order MoSi2Powder.
2. MoSi according to claim 12Based composites, which is characterized in that the average grain of the ball shaped nano Cu particle Diameter is within the scope of 40~50nm.
3. MoSi according to claim 12Based composites, which is characterized in that the MoSi2The average grain diameter of powder is 1.3um, the nano Si3N4The average grain diameter of powder is 100nm.
4. a kind of novel Si3N4Enhance MoSi2The preparation method of based composites, which comprises the following steps:
(1) 20~30 parts of nano Si is weighed3N4Powder is placed in ball grinder together with 50 parts of dehydrated alcohols, under nitrogen protection 1~3h of ball milling is carried out, later, 2~5 parts of gamma-aminopropyl-triethoxy-silane coupling agent is added, continues 2~4h of ball milling, use The mixed solvent being made of in equal volume deionized water and dehydrated alcohol is to the nano Si for wrapping up in slurry3N4Powder carries out 3~6 washings；
(2) by the above-mentioned nano Si for wrapping up in slurry3N4Powder is added in the reactor equipped with magnetic stirring apparatus, and adds into reactor Enter the mixed solvent that 200mL is made of in equal volume deionized water and dehydrated alcohol, in the magnetic agitation that revolving speed is 120~180rpm Under, 5~8 parts of ball shaped nano Cu particle is added in reactor, 1~3h of magnetic agitation under 300~500rpm is switched to, later, Centrifugal treating is carried out, the nano Si that surface uniform load has nano Cu particle is prepared3N4Powder；
(3) 8~10 parts of polyvinyl alcohol are dissolved in the deionized water that 20 parts of temperature are 100 DEG C, stirring is prepared to being completely dissolved Obtain poly (vinyl alcohol) binder；
(4) mixed solvent being made of 600mL deionized water and 400mL dehydrated alcohol is added to equipped with high-speed stirring apparatus and In the reactor of heating device, in the case where revolving speed is 500~800rpm stirring, first the poly (vinyl alcohol) binder of above-mentioned preparation is added Into reactor, then slowly by the micron order MoSi of 60~70g2Powder is added in reactor, finally by the table of above-mentioned preparation Face uniform load has the nano Si of nano Cu particle3N4Powder is added in reactor, later, switch to temperature be 100~120 DEG C, Rate is that 2~4h is reacted under 800~1000rpm, obtains being distributed uniform mixed slurry；
(5) the uniform mixed slurry of above-mentioned distribution is fitted into etc. in static pressure rubber mold, is pressed under 65~80MPa pressure Type, then be placed in the vacuum drying oven that preheating temperature is 600~800 DEG C, with the heating rate of 5 DEG C/min, it is warming up to 1850~1900 DEG C, and 4h is kept the temperature under 1850~1900 DEG C, 10MPa, and later with the annealing rate of 5 DEG C/min, taking-up when being cooled to room temperature, system It is standby to obtain novel Si3N4Enhance MoSi2Based composites.
CN201910504812.2A 2019-06-12 2019-06-12 A kind of novel Si3N4Enhance MoSi2Based composites and preparation method Pending CN110183233A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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