CN101708989B - Method for preparing aluminum nitride/boron nitride composite ceramic through combustion synthesis method - Google Patents
Method for preparing aluminum nitride/boron nitride composite ceramic through combustion synthesis method Download PDFInfo
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- CN101708989B CN101708989B CN2009100734131A CN200910073413A CN101708989B CN 101708989 B CN101708989 B CN 101708989B CN 2009100734131 A CN2009100734131 A CN 2009100734131A CN 200910073413 A CN200910073413 A CN 200910073413A CN 101708989 B CN101708989 B CN 101708989B
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Abstract
A method for preparing aluminum nitride/boron nitride composite ceramic through combustion synthesis method relates to a method for preparing composite ceramic. The invention solves the problem that the current method for preparing aluminum nitride/boron nitride composite ceramic has high energy consumption, long production period and low production efficiency. The method comprises the following steps: performing ball milling to the dried raw material in a mixing bowl to obtain power, then pressing power to prepare blank, then placing the blank in a high pressure reactor, filling nitrogen, igniting to perform a self-propagation combustion reaction and obtaining aluminum nitride/boron nitride composite ceramic after the self-propagation combustion reaction. The method of the invention adopts the chemical energy so as to save a great deal of energy, and the reaction process for synthesizing the aluminum nitride/boron nitride composite ceramic only needs several minutes so as to increase the production efficiency. The bending strength of the aluminum nitride/boron nitride composite ceramic obtained by the method of the invention is 60MPa-800MPa and the fracture toughness is 2Mpam<-1/2>-9Mpam<-1/2>.
Description
Technical field
The present invention relates to a kind of method for preparing composite ceramics.
Background technology
Hot pressing sintering method prepares the long heating and the cooling time (being generally several hours even tens hours) of method needs of aluminium nitride/boron nitride composite ceramics at present, and needs following process, makes that the production efficiency of this method is lower, and power consumption.With the composite powder that obtains BN wrapping portion AlN behind boric acid, urea and the aluminium nitride AlN powder mix reduction nitridation; Again composite powder is made the method for AlN-BN composite ceramic material through sintering; Because the more oxygen impurities that in the course of processing of composite powder, induced one, thereby reduced the performance of AlN-BN composite ceramics.
Summary of the invention
Technical problem to be solved by this invention is in order to solve the existing problem that the method energy consumption is high, the production cycle is long, production efficiency is low for preparing the aluminium nitride/boron nitride composite ceramics, to provide a kind of combustion synthesis method to prepare the method for aluminium nitride/boron nitride composite ceramics.
The method that combustion synthesis method of the present invention prepares the aluminium nitride/boron nitride composite ceramics is following: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10～20 hours; Then 0～100 weight part raw material a and 0～100 weight part raw material b were put into the mixing tank ball milling 20 hours～25 hours; Obtain powder, wherein the weight part number average of raw material a and raw material b is not 0 part; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 30MPa～200MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2, TiN, TiCN, TiC, ZrB
2, one or more and aluminium powder among ZrC, NbC, NbN, TaN and the TaC form, the weight percent of aluminium powder is 20%～80% among the raw material a; The b of raw material described in the step 1 is made up of a kind of and norbide in silica flour and titanium valve mixture, titanium valve and the silica flour, and the molar percentage of norbide is 50% among the raw material b.
The inventive method can also be in step 1 with raw material a, raw material b and thinner respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10 hours～20 hours, will pass through exsiccant raw material a, raw material b and thinner then and put into the mixing tank ball milling 20 hours～25 hours, obtain mixed powder; The parts by weight of raw material a are 0～100 part in the step 1, and raw material b parts by weight are 0～100 part, and the thinner parts by weight are 0～70 part, and raw material a, raw material b and thinner weight part number average are not 0 part; Thinner described in the step 1 is ceramic-like thinner or metal species thinner; Described metal species thinner is one or more the combination among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta; Described ceramic-like thinner is BN, AlN, SiC, HfC, C, ZrC, TiC, B
4C, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, Mo Laishi and TiO
2In one or more combination; Described ceramic-like thinner C is decolorizing carbon, graphite, diamond, thomel, carbon nanotube or bucky-ball.
It is following that the present invention prepares the chemical reaction that the method for aluminium nitride/boron nitride composite ceramics utilizes:
x(Al+yTiB
2)+B
4C+Si+(2+0.5x)N
2＝x(AlN+yTiB
2)+4BN+SiC
Through control x, control the content of aluminium nitride AlN phase in the aluminium nitride/boron nitride composite ceramics in the formula.
The inventive method is utilized the chemical energy of raw material; Only need to accomplish reaction after the very little energy igniting; Thereby practice thrift a large amount of energy, and reduce the cost of product, and the reaction process of synthetic aluminium nitride AlN/SP 1 composite ceramics only needs several minutes; Improved production efficiency; High temperature (temperature can reach 2000 ℃～4000 ℃) in the synthetic aluminium nitride AlN of burning/SP 1 composite ceramics process helps the volatilization of impurity, thereby adopts the purity of the aluminium nitride/boron nitride composite ceramics that the inventive method obtains very high, excellent property.The high temperature that is produced in the synthetic aluminium nitride AlN of burning/SP 1 composite ceramics process; Make TiB2 and aluminium liquid have good wettability; But forced fluid phase sintering effect on the one hand; Improve the density of aluminium nitride/boron nitride composite ceramics, can improve the speed of reaction of aluminium on the other hand, improve the transformation efficiency of aluminium nitride/boron nitride composite ceramics.Some other material also has the characteristic similar with TiB2, at high temperature has good wettability with aluminium liquid, like TiN, TiCN, TiC, ZrB
2, ZrC, NbC, NbN, TaN and TaC.Adopting the bending strength of the inventive method gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10～20 hours; Then 0～100 weight part raw material a and 0～100 weight part raw material b were put into the mixing tank ball milling 20 hours～25 hours; Obtain powder, wherein the weight part number average of raw material a and raw material b is not 0 part; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 30MPa～200MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2, TiN, TiCN, TiC, ZrB
2, one or more and aluminium powder among ZrC, NbC, NbN, TaN and the TaC form, the weight percent of aluminium powder is 20%～80% among the raw material a; The b of raw material described in the step 1 is made up of titanium valve or silica flour and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～400MPa, and fracture toughness property is 2MPam
-1/2～5MPam
-1/2
Embodiment two: what this embodiment and embodiment one were different is in the step 1 mixture of 0.1～100 weight part raw material a and 0.1～100 weight part raw material b to be put into the mixing tank ball milling.Other is identical with embodiment one.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～400MPa, and fracture toughness property is 2MPam
-1/2～5MPam
-1/2
Embodiment three: this embodiment and embodiment one are different, and to be the b of raw material described in the step 1 be made up of silica flour and titanium valve mixture and norbide, and the molar percentage of norbide is 50% among the raw material b.Other is identical with embodiment one.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 70MPa～400MPa, and fracture toughness property is 2MPam
-1/2～5MPam
-1/2
In silica flour described in this embodiment and the titanium valve mixture silica flour and titanium valve be arbitrarily than.
Embodiment four: this embodiment and embodiment one are different be in the step 1 with raw material a, raw material b and thinner respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10 hours～20 hours, will pass through exsiccant raw material a, raw material b and thinner then and put into the mixing tank ball milling 20 hours～25 hours, obtain mixed powder; The parts by weight of raw material a are 0～100 part in the step 1, and raw material b parts by weight are 0～100 part, and the thinner parts by weight are 0～70 part, and raw material a, raw material b and thinner weight part number average are not 0 part; Thinner described in the step 1 is ceramic-like thinner or metal species thinner; Described metal species thinner is one or more the combination among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta; Described ceramic-like thinner is BN, AlN, SiC, HfC, C, ZrC, TiC, B
4C, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, Mo Laishi and TiO
2In one or more combination; Described ceramic-like thinner C is decolorizing carbon, graphite, diamond, thomel, carbon nanotube or bucky-ball.Other is identical with embodiment one.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 65MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment five: this embodiment and embodiment four are different be in the step 1 with raw material b and thinner respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10 hours～20 hours, will pass through exsiccant raw material b and thinner then and put into the mixing tank ball milling 20 hours～25 hours, obtain mixed powder; Raw material b parts by weight are 0.1～100 part in the step 1, and the thinner parts by weight are 0.1～70 part; The b of raw material described in the step 1 is made up of a kind of and norbide in silica flour or the titanium valve, and the molar percentage of norbide is 50% among the raw material b.Other is identical with embodiment four.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment six: this embodiment and embodiment five are different, and to be the b of raw material described in the step 1 be made up of silica flour and titanium valve mixture and norbide, and the molar percentage of norbide is 50% among the raw material b.Other is identical with embodiment five.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 70MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
In silica flour described in this embodiment and the titanium valve mixture silica flour and titanium valve be arbitrarily than.
Embodiment seven: this embodiment and embodiment four are different be in the step 1 with raw material a, raw material b and thinner respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10 hours～20 hours, will pass through exsiccant raw material a, raw material b and thinner then and put into the mixing tank ball milling 20 hours～25 hours, obtain mixed powder; The parts by weight of raw material a are 0.1～100 part in the step 1, and raw material b parts by weight are 0.1～100 part, and the thinner parts by weight are 0.1～70 part; The a of raw material described in the step 1 is by TiB
2, TiN, TiCN, TiC, ZrB
2, a kind of among ZrC, NbC, NbN, TaN and the TaC form with aluminium powder, the weight percent of aluminium powder is 20%～80% among the raw material a; The b of raw material described in the step 1 is made up of a kind of and norbide in silica flour or the titanium valve, and the molar percentage of norbide is 50% among the raw material b.Other is identical with embodiment four.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment eight: what this embodiment and embodiment seven were different is that the b of raw material described in the step 1 is made up of silica flour, titanium valve and norbide, and the molar percentage of norbide is 50% among the raw material b.Other is identical with embodiment seven.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment nine: what this embodiment and embodiment four～eight were different is that the thinner described in the step 1 is ceramic-like thinner or metal species thinner.Other is identical with embodiment four～eight.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment ten: this embodiment and embodiment nine are different is that the metal species thinner described in the step 1 is one or more the combination among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta.Other is identical with embodiment nine.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPam～800MPa, and fracture toughness property is 3MPam
-1/2～9MPam
-1/2
Embodiment 11: what this embodiment and embodiment nine were different is that the ceramic-like thinner described in the step 1 is BN, AlN, SiC, HfC, C, ZrC, TiC, B
4C, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, Mo Laishi and TiO
2In one or more combination.Other is identical with embodiment nine.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment 12: what this embodiment and embodiment 11 were different is that the ceramic-like thinner C described in the step 1 is decolorizing carbon, graphite, diamond, thomel, carbon nanotube or bucky-ball.Other is identical with embodiment 11.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～800MPa, and fracture toughness property is 2MPam
-1/2～9MPam
-1/2
Embodiment 13: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material b in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10 hours～20 hours, then 100 weight part raw material b are put into the mixing tank ball milling 20 hours～25 hours, obtain powder; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 50MPa～200MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The b of raw material described in the step 1 is made up of a kind of and norbide in silica flour, titanium valve and silica flour and the titanium valve mixture, and the molar percentage of norbide is 50% among the raw material b.
In silica flour described in this embodiment and the titanium valve mixture silica flour and titanium valve be arbitrarily than.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 60MPa～120MPa, and fracture toughness property is 2MPam
-1/2～3.5MPam
-1/2
Embodiment 14: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and thinner respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10～20 hours, then 75 weight part raw material a and 25 parts by weight diluent are put into the mixing tank ball milling 20 hours～25 hours, obtain powder; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 30MPa～200MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2Form with aluminium powder, the weight percent of aluminium powder is 60% among the raw material a; Thinner described in the step 1 is BN.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 180MPa～200MPa, and fracture toughness property is 2.1MPam
-1/2～3MPam
-1/2
Embodiment 15: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10～20 hours, then 10 weight part raw material a and 90 weight part raw material b are put into the mixing tank ball milling 20 hours～25 hours, obtain powder; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2Form with aluminium powder, the weight percent of aluminium powder is 50% among the raw material a; The b of raw material described in the step 1 is made up of silica flour and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 80MPa～130MPa, and fracture toughness property is 2MPam
-1/2～2.8MPam
-1/2
Embodiment 16: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10～20 hours, then 20 weight part raw material a and 80 weight part raw material b are put into the mixing tank ball milling 20 hours～25 hours, obtain powder; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 110MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2Form with aluminium powder, the weight percent of aluminium powder is 50% among the raw material a; The b of raw material described in the step 1 is made up of silica flour and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 100MPa～140MPa, and fracture toughness property is 2.6MPam
-1/2～3MPam
-1/2
Embodiment 17: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 10～20 hours, then 30 weight part raw material a and 70 weight part raw material b are put into the mixing tank ball milling 24 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 90MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2Form with aluminium powder, the weight percent of aluminium powder is 80% among the raw material a; The b of raw material described in the step 1 is made up of silica flour and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 120MPa～150MPa, and fracture toughness property is 2MPam
-1/2～4MPam
-1/2
Embodiment 18: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 15 hours, then 50 weight part raw material a and 50 weight part raw material b are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2Form with aluminium powder, the weight percent of aluminium powder is 70% among the raw material a; The b of raw material described in the step 1 is made up of titanium valve and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 140MPa～180MPa, and fracture toughness property is 2MPam
-1/2～4MPam
-1/2
Embodiment 19: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 18 hours, then 30 weight part raw material a and 70 weight part raw material b are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is made up of TiN and aluminium powder, and the weight percent of aluminium powder is 60% among the raw material a; The b of raw material described in the step 1 is made up of silica flour and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 130MPa～180MPa, and fracture toughness property is 2MPam
-1/2～4MPam
-1/2
Embodiment 20: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and raw material b, BN respectively in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 18 hours, then 60 weight part raw material a, 20 weight part raw material b and 20 weight part BN are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is made up of TiN and aluminium powder, and the weight percent of aluminium powder is 70% among the raw material a; The b of raw material described in the step 1 is made up of silica flour and norbide, and the molar percentage of norbide is 50% among the raw material b.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 120MPam～180MPa, and fracture toughness property is 2.4MPam
-1/2～4MPam
-1/2
Embodiment 21: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 18 hours, then 100 weight part raw material a are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is made up of TiN and aluminium powder, and the weight percent of aluminium powder is 70% among the raw material a.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 300MPam～400MPa, and fracture toughness property is 4MPam
-1/2～5MPam
-1/2
Embodiment 22: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 18 hours, then 80 weight part raw material a are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is made up of TiN and aluminium powder, and the weight percent of aluminium powder is 70% among the raw material a.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 200MPam～260MPa, and fracture toughness property is 3MPam
-1/2～4MPam
-1/2
Embodiment 23: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 18 hours, then 100 weight part raw material a are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is made up of TiN and aluminium powder, and the weight percent of aluminium powder is 70% among the raw material a.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 300MPam～400MPa, and fracture toughness property is 4MPam
-1/2～6MPam
-1/2
Embodiment 24: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and SiC whisker respectively in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 18 hours, then 95 weight part raw material a and 5 weight part SiC whiskers are put into the mixing tank ball milling 22 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2Form with aluminium powder, the weight percent of aluminium powder is 70% among the raw material a.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 600MPam～800MPa, and fracture toughness property is 7MPam
-1/2～9MPam
-1/2
Embodiment 25: to prepare the method for aluminium nitride/boron nitride composite ceramics following for combustion synthesis method in this embodiment: one, with raw material a and carbon nanotube respectively in vacuum tightness less than 10
-3Atm, temperature are under 100 ℃ of conditions dry 19 hours, then 95 weight part raw material a and 5 weight part carbon nanotubes are put into the mixing tank ball milling 23 hours, obtain powder; Two, powder compression being become porosity is 40% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 100MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is made up of TiC and aluminium powder, and the weight percent of aluminium powder is 70% among the raw material a.
The bending strength of this embodiment gained aluminium nitride/boron nitride composite ceramics is 700MPam～800MPa, and fracture toughness property is 7MPam
-1/2～9MPam
-1/2
Claims (6)
1. combustion synthesis method prepares the method for aluminium nitride/boron nitride composite ceramics, and it is following to it is characterized in that combustion synthesis method prepares the method for aluminium nitride/boron nitride composite ceramics: one, with raw material a and raw material b respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10～20 hours; Then 0～100 weight part raw material a and 0～100 weight part raw material b were put into the mixing tank ball milling 20 hours～25 hours; Obtain powder, wherein the weight part number average of raw material a and raw material b is not 0 part; Two, powder compression being become porosity is 35%～45% blank; Three, the blank of step 2 gained is put into high-pressure reactor; The pressure that charges in nitrogen to the high pressure reactor drum is 30MPa～200MPa, then in the centerfire of blank upper surface, the self-propagating combustion reaction takes place; The self-propagating combustion reaction finishes, and promptly gets the aluminium nitride/boron nitride composite ceramics; The a of raw material described in the step 1 is by TiB
2, one or more and aluminium powder among TiN, TiCN, TiC, ZrB2, ZrC, NbC, NbN, TaN and the TaC form, the weight percent of aluminium powder is 20%～80% among the raw material a; The b of raw material described in the step 1 is made up of a kind of and norbide in silica flour and titanium valve mixture, titanium valve and the silica flour, and the molar percentage of norbide is 50% among the raw material b.
2. the described combustion synthesis method of claim 1 prepares the method for aluminium nitride/boron nitride composite ceramics, it is characterized in that in the step 1 raw material a, raw material b and thinner respectively in vacuum tightness less than 10
-3Atm, temperature are under 80 ℃～120 ℃ conditions dry 10 hours～20 hours, will pass through exsiccant raw material a, raw material b and thinner then and put into the mixing tank ball milling 20 hours～25 hours, obtain mixed powder; The parts by weight of raw material a are 0～100 part in the step 1, and raw material b parts by weight are 0～100 part, and the thinner parts by weight are 0～70 part, and raw material a, raw material b and thinner weight part number average are not 0 part.
3. combustion synthesis method according to claim 2 prepares the method for aluminium nitride/boron nitride composite ceramics, it is characterized in that the thinner described in the step 1 is ceramic-like thinner or metal species thinner.
4. combustion synthesis method according to claim 3 prepares the method for aluminium nitride/boron nitride composite ceramics, it is characterized in that the metal species thinner described in the step 1 is one or more the combination among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta.
5. combustion synthesis method according to claim 3 prepares the method for aluminium nitride/boron nitride composite ceramics, it is characterized in that the ceramic-like thinner described in the step 1 is BN, AlN, SiC, HfC, C, ZrC, TiC, B
4C, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, Mo Laishi and TiO
2In one or more combination.
6. combustion synthesis method according to claim 5 prepares the method for aluminium nitride/boron nitride composite ceramics, it is characterized in that the ceramic-like thinner C described in the step 1 is decolorizing carbon, graphite, diamond, thomel, carbon nanotube or bucky-ball.
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| CN102584245B (en) * | 2012-02-21 | 2013-07-10 | 东北大学 | Preparation method of aluminium nitride and titanium diboride composite ceramic |
| CN103288436B (en) * | 2013-05-31 | 2014-10-08 | 哈尔滨工业大学 | Method for synthetizing fused cast by combustion of MgAl2O4 ceramic |
| CN103274680B (en) * | 2013-05-31 | 2014-10-08 | 哈尔滨工业大学 | Method for casting Y3Al5O12 ceramics by combustion synthesis |
| CN104211062B (en) * | 2014-09-05 | 2016-05-04 | 哈尔滨工业大学 | A kind of non-oxidized substance eutectic ceramic amorphous powder reactive spray preparation method |
| CN104725049B (en) * | 2015-03-23 | 2017-03-15 | 北京科技大学 | A kind of preparation method of aluminium nitride/boron nitride composite ceramic powder |
| CN105016737B (en) * | 2015-07-08 | 2017-10-13 | 青岛桥海陶瓷新材料科技有限公司 | Combustion synthesis method produces the preparation method of aluminium nitride and nitridation silica hybrid material |
| CN106365641B (en) * | 2016-08-23 | 2018-12-11 | 安徽科创中光科技有限公司 | Method for synthesizing silicon nitride and aluminum nitride at one time |
| CN112759402A (en) * | 2021-03-16 | 2021-05-07 | 福建臻璟新材料科技有限公司 | Preparation process of high-strength black aluminum nitride ceramic |
| CN113149658B (en) * | 2021-04-28 | 2023-02-07 | 武汉理工大学 | Titanium nitride-based composite ceramic material and preparation method thereof |
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