CN101734916B - Boron nitride-titanium diboride ceramic composite material and preparation method thereof - Google Patents
Boron nitride-titanium diboride ceramic composite material and preparation method thereof Download PDFInfo
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- CN101734916B CN101734916B CN 200910073414 CN200910073414A CN101734916B CN 101734916 B CN101734916 B CN 101734916B CN 200910073414 CN200910073414 CN 200910073414 CN 200910073414 A CN200910073414 A CN 200910073414A CN 101734916 B CN101734916 B CN 101734916B
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Abstract
The invention relates to a boron nitride-titanium diboride ceramic composite material and a preparation method thereof. The invention solves the problems that preparation of the traditional boron nitride-based ceramic composite material has high cost, long production period and difficulty in manufacturing products with large size. The boron nitride-titanium diboride ceramic composite material is prepared from carbonized boron powder, titanium powder and diluent powder. The boron nitride-titanium diboride ceramic composite material is prepared by the following steps of raw material drying, ball milling and mixing, blank production and self-propagating synthesis of the blank. The method has short production period and low cost ad can realize the production of products with large size.
Description
Technical field
The present invention relates to a kind of preparation method of boron nitride-based ceramic composite material.
Background technology
Boron nitride (BN) goods have high temperature resistant, corrosion-resistant, electrical insulation capability, and good heat-shock resistance and processability, thereby get a lot of applications in industry.Utilize BN to nonwetting and anti-the invading property of glass, metal melt, in special smelting, make the parts such as crucible, vessel, passage, transferpump of the multiple non-ferrous metal of melting, precious metal and rare metal; Found the vessel of boron single crystal; When making thin-film capacitor and cigarette wrapping paper, can receive the effect of high-quality high yield as molten aluminum evaporation vessel with BN; The BN goods also can be used as the mould of cast steel and cast glass.Can be as the high-temperature insulation parts of Plasma Welding instrument, the lining of multiple well heater, the lining of rocket chamber, the heatshield material of spaceship, the protective casing of pyrometer couple etc.
The BN goods can easily carry out mechanical workout; and working accuracy is very high; therefore greatly enlarge its range of application and improved use value; for example, the ring-type high-temperature insulation dissection type protective guard part used of the radiating pipe on the high frequency traveling-wave tube collector, Novel welding machine; not only complex-shaped; and dimension precision requirement is high, and general oxide ceramics both had been difficult to figuration manufacture and had lacked desirable thermal shock resistance, and just can the two all was met with the BN ceramic.Therefore the BN stupalith has good market outlook.
The boron nitride-base conductivity ceramics is the good candidate materials of evaporation boat.Conductive evaporation boat is the crucial consumable material of vacuum plating industry.In the approximately 12 hours work-ing life of import evaporation boat, evaporation boat is as disposable easily-consumed products, and annual requirement is hundreds of hundred million, has wide market outlook.In the metal evaporation industry, first-generation evaporation boat material is graphite, but it is easily corroded by liquid aluminium, and the life-span is very short.After the graphite surface coating resembled the supercoat of TiC, HfC, TaC etc., the life-span of graphite boat also only had several hours afterwards.Present industrial main application BN-TiB
2S-generation evaporation boat material is in conjunction with solidity to corrosion and the TiB of BN to aluminium liquid
2Excellent conductive capability, have good use properties.
At present the traditional preparation technology of boron nitride-base ceramic material mainly contains: normal pressure-sintered, hot pressed sintering, HIP sintering method and microwave sintering are high warm with the long high temperature of the normal pressure-sintered needs of plasma agglomeration, consume energy very large, and cost is high; Hot pressed sintering resulting product simple shape generally needs several hours, and the production cycle is long, and cost is higher; And the HIP sintering performance is good, but cost of manufacture is higher; Microwave sintering and plasma sintering equipment are complicated, are difficult to make the large size product.
Summary of the invention
The cost that exists in the existing boron nitride-base ceramic material preparation is high, the production cycle long and make large-sized product hard problem in order to solve in the present invention, and the preparation method of boron nitride-titanium diboride ceramic composite material is provided.
Boron nitride-titanium diboride ceramic composite material is made by 20%～80% boron carbide powder, 10%～70% titanium valve and 0%～70% thinner powder according to weight percent.
The boron nitride based composite ceramic ceramic composite is made according to following steps: one, raw material drying: release the agent powder according to what weight percent took by weighing respectively 20%～80% boron carbide powder, 10%～70% titanium valve and 0%～70%, and then the raw material that takes by weighing placed respectively under 80～150 ℃ the vacuum condition dry 8～12h; Two, raw material after the drying is put into ball mill and carried out the ball milling mixing, rotational speed of ball-mill is 50～200r/min, and Ball-milling Time is 12～24h, and ball material mass ratio is 3: 1; Three, the mixture behind the ball milling is packed in rubber bag or the latex rubber bag, cold isostatic compaction obtains blank, and pressure is 8～30MPa, the porosity 35%～45% of blank; Four, blank is put into the seal-off pressure container that is connected with recirculated water, then be filled with nitrogen and make the pressure in the seal-off pressure container reach 30～200MPa, igniting, the raw material self-propagating combustion namely prepares boron nitride-titanium carbonitride composite ceramic material.
The reaction principle of boron nitride-titanium diboride ceramic composite material of the present invention preparation is: preparation method of the present invention adopts combustion synthesis method, i.e. self propagating high temperature synthetic (the English SHS that is called for short) is a kind of preparation technology of novel inorganic refractory.A large amount of reaction heat that it is emitted when utilizing the raw material building-up reactions make reaction from keeping down until react end, thereby obtain a kind of method of required product.
The synthetic chemical reaction that boron nitride-the titanium carbonitride ceramic composite utilizes of burning is:
B
4C+Ti+2N
2＝4BN+TiC (1)
Titanium valve is suitably excessive in the raw material, can generate the titanium nitride ceramic composition, and itself and product titanium carbide combine, and forms titanium carbonitride.
2Ti+N
2＝2TiN (2).
TiC+TiN＝TiCN (3)
B in the raw material
4C is suitably excessive, can generate the BN-C composition, has important application as that high temperature material.
B
4C+2N
2＝4BN+C (4)
Combustion synthesis reaction of the present invention carries out under high pressure nitrogen.The rising of atmosphere pressures is conducive to react to such an extent that fully carry out, and suppresses aluminium nitride and boron nitride decomposition at high temperature.Pressure values is desirable: 30～200MPa.Higher pressure is also passable, but the effect raising is not remarkable, and waste nitrogen and the energy, increases the danger of producing.
The advantage of boron nitride-titanium diboride ceramic composite material of the present invention is as follows:
1, preparation method's of the present invention reaction process only needs several minutes to finish, and has greatly improved production efficiency, has shortened the production cycle, and preparation method of the present invention is with short production cycle;
2, the present invention is with cheap norbide (B
4C) be raw material, with combustion reactions B
4C+Ti+2N
2=4BN+SiC is the basis, the synthetic boron nitride based composite ceramic of burning, and the present invention needs very little energy igniting to get final product, can save a large amount of energy, greatly and reduce the cost of product, preparation method of the present invention and existing boron nitride-base ceramic material preparation method have been compared cost 30%～50%;
3, preparation method of the present invention can make large-sized product (diameter is that 40～200mm, length are 50～1000mm); The inventive method is utilized raw material self extensive chemical exothermic heat of reaction, do not need complicated high-temperature heating equipment, synthesising reacting time is short, and is lower to the requirement of refrigerating unit, simple in equipment, the manufacturing of large size equipment, processing are relatively easily, and what the inventive method adopted is combustion synthesis method, in conjunction with without the hot isostatic pressing method of sealing, does not need complicated wrapper technology, simultaneously product is stressed evenly, has realized the preparation of large size, complicated shape pottery.
4, boron nitride of the present invention-titanium carbonitride composite ceramic material excellent performance.Temperature is very high in the reaction process of the inventive method, can reach 2000～3000 ℃, implement simultaneously the hot isostatic pressing of high pressure, need not to add low-melting sintering aid, boron nitride of the present invention-titanium carbonitride composite ceramic material is pure ceramic product, without the low melting point Grain-Boundary Phase, high-temperature behavior is outstanding, and the use temperature of boron nitride of the present invention-titanium carbonitride composite ceramic material can reach more than 2500 ℃; Method of the present invention can make product have different conductivities by regulating the content of titanium carbonitride in the product, as the high-temperature electric conduction material; Boron nitride of the present invention-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, hundreds of times of room temperature-1000 ℃ cold cycling, and product is without damage.Product has good processability, adopts different lathes all can process; The bending strength of boron nitride of the present invention-titanium carbonitride composite ceramic material can reach 60～150MPa, and the bending strength under 2000 ℃ of hot conditionss can reach 40～90MPa.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the present embodiment boron nitride-titanium diboride ceramic composite material is made by 20%～80% boron carbide powder, 10%～70% titanium valve and 0%～70% thinner powder according to weight percent.
Boron carbide powder in the present embodiment, titanium valve all be purchase in market available.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, hundreds of times of room temperature-1000 ℃ cold cycling, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 60～150MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment one: the present embodiment boron nitride-titanium diboride ceramic composite material is made by 30%～60% boron carbide powder, 20%～50% titanium valve and 0%～60% thinner powder according to weight percent.
Embodiment two: present embodiment and embodiment one are different, and to be boron nitride-titanium diboride ceramic composite material made by 30%～70% boron carbide powder, 10%～60% titanium valve and 10%～60% thinner powder according to weight percent.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different, and to be boron nitride-titanium diboride ceramic composite material made by 30%～60% boron carbide powder, 20%～50% titanium valve and 20%～50% thinner powder according to weight percent.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different, and to be boron nitride-titanium diboride ceramic composite material made by 50% boron carbide powder, 40% titanium valve and 10% thinner powder according to weight percent.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one to four were different is that the thinner powder is ceramic-like thinner powder and/or metal species thinner powder.Other is identical with embodiment one to four.
When the thinner powder is mixture in the present embodiment, can be mixed by any ratio between various thinner powder.
Embodiment six: what present embodiment and embodiment five were different is that ceramic-like thinner powder is by BN, AlN, SiC, HfC, C, ZrC, TiC, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, Mo Laishi and TiO
2In a kind of or several compositions wherein.Other is identical with embodiment five.
When ceramic-like thinner powder is mixture in the present embodiment, can be mixed by any ratio between various ceramic-like thinner powder.
Embodiment seven: present embodiment and embodiment five are different is metal species thinner powder by a kind of among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta or several composition the wherein.Other is identical with embodiment five.
When metal species thinner powder is mixture in the present embodiment, can be mixed by any ratio between various metal species thinner powder.
Embodiment eight: present embodiment and embodiment one to seven are different, and to be boron nitride-titanium diboride ceramic composite material made by 63% boron carbide powder, 32% titanium valve and 5% boron nitride according to weight percent.Other is identical with embodiment one to seven.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2500 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 400 times, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 70～140MPa, and bending strength can reach 50～80MPa under 2000 ℃ of hot conditionss.
Embodiment nine: present embodiment and embodiment one to seven are different, and to be boron nitride-titanium diboride ceramic composite material made by 59% boron carbide powder, 31% titanium valve and 10% boron nitride according to weight percent.Other is identical with embodiment one to seven.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2500 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 60～140MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Embodiment ten: present embodiment and embodiment one to seven are different, and to be boron nitride-titanium diboride ceramic composite material made by 26% boron carbide powder, 14% titanium valve and 60% boron nitride according to weight percent.Other is identical with embodiment one to seven.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 400 times, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 70～150MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment 11: present embodiment and embodiment one to seven are different, and to be boron nitride-titanium diboride ceramic composite material made by 33% boron carbide powder, 17% titanium valve and 50% boron nitride according to weight percent.Other is identical with embodiment one to seven.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 400 times, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 80～150MPa, and bending strength can reach 70～90MPa under 2000 ℃ of hot conditionss.
Embodiment 12: present embodiment and embodiment one to seven are different, and to be boron nitride-titanium diboride ceramic composite material made by 32% boron carbide powder, 16% titanium valve and 53% Cr according to weight percent.Other is identical with embodiment one to seven.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 70～120MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 13: present embodiment and embodiment one to seven are different, and to be boron nitride-titanium diboride ceramic composite material made by 35% boron carbide powder, 22% titanium valve and 43% TiC according to weight percent.Other is identical with embodiment one to seven.
The boron nitride of present embodiment-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 600 times, and product is without damage; The boron nitride of present embodiment-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride of present embodiment-titanium carbonitride composite ceramic material can reach 60～140MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Embodiment 14: the present embodiment boron nitride-titanium diboride ceramic composite material is made according to following steps: one, raw material drying: release the agent powder according to what weight percent took by weighing respectively 20%～80% boron carbide powder, 10%～70% titanium valve and 0%～70%, and then the raw material that takes by weighing placed respectively under 80～150 ℃ the vacuum condition dry 8～12h; Two, raw material after the drying is put into ball mill and carried out the ball milling mixing, rotational speed of ball-mill is 100～200r/min, and Ball-milling Time is 12～24h, and ball material mass ratio is 3: 1; Three, the mixture behind the ball milling is packed in rubber bag or the latex rubber bag, cold isostatic compaction obtains blank, and pressure is 15～30MPa, the porosity 35%～45% of blank; Four, blank is put into the seal-off pressure container that is connected with recirculated water, then be filled with nitrogen and make the pressure in the seal-off pressure container reach 30～200MPa, igniting, the raw material self-propagating combustion namely prepares boron nitride-titanium carbonitride composite ceramic material.
Boron carbide powder in the present embodiment step 1, titanium valve all be purchase in market available.
Vacuum tightness is less than 10 in the vacuum-drying of present embodiment step 1
2Pa.
Resulting blank diameter is that 40～200mm, length are 50～1000mm in the present embodiment step 3.
Igniting in the present embodiment step 4 can be adopted the Ni-Cr resistance wire, and priming mixture has a variety of, simply can adopt granularity less than the mixture of the pure Ti powder of 300 orders and carbon black, and pure Ti powder and carbon black can be mixed by any ratio.。
Self-propagating combustion in the present embodiment step 4 is recorded in the article of a piece " self-propagating combustion material synthesis technology " by name delivering on Zheng's bodyguard in 1999 " Shandong pottery " far away.
Present embodiment can be made large size, and (diameter is that 40～200mm, length are 50～1000mm) boron nitride-titanium carbonitride composite ceramic material.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, hundreds of times of room temperature-1000 ℃ cold cycling, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～150MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment 15: what present embodiment and embodiment 14 were different is to take by weighing 30%～60% boron carbide powder, 20%～50% titanium valve and 0%～60% thinner powder according to weight percent in the step 1.Other step and parameter are identical with embodiment 14.
Embodiment 16: present embodiment and embodiment 14 are different be in the step 1 according to weight percent by 30%～60% boron carbide powder, 20%～50% titanium valve and 20%～50% thinner powder.Other step and parameter are identical with embodiment 14.
Embodiment 17: present embodiment and embodiment 14 are different, and to be boron nitride-titanium diboride ceramic composite material made by 50% boron carbide powder, 40% titanium valve and 40% thinner powder according to weight percent.Other step and parameter are identical with embodiment 14.
Embodiment 18: what present embodiment and embodiment 14 to 17 were different is that the thinner powder is ceramic-like thinner powder and/or metal species thinner powder in the step 1.Other step and parameter are identical with embodiment 14 to 17.
When the thinner powder is mixture in the present embodiment, can be mixed by any ratio between various thinner powder.
Embodiment 19: what present embodiment and embodiment 18 were different is that ceramic-like thinner powder is by BN, AlN, SiC, HfC, C, ZrC, TiC, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, Mo Laishi and TiO
2In a kind of or several compositions wherein.Other step and parameter are identical with embodiment 18.
When ceramic-like thinner powder is mixture in the present embodiment, can be mixed by any ratio between various ceramic-like thinner powder.
Embodiment 20: present embodiment and embodiment 18 are different is metal species thinner powder by a kind of among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta or several composition the wherein.Other step and parameter are identical with embodiment 18.
When metal species thinner powder is mixture in the present embodiment, can be mixed by any ratio between various metal species thinner powder.
Embodiment 21: what present embodiment and embodiment 14 were different is that boron nitride-titanium diboride ceramic composite material is made according to following steps: one, raw material drying: release the agent powder according to what weight percent took by weighing respectively 20%～80% boron carbide powder, 10%～70% titanium valve and 0%～70%, and then the raw material that takes by weighing placed respectively under 100 ℃ the vacuum condition dry 12h; Two, raw material after the drying is put into ball mill and carried out the ball milling mixing, rotational speed of ball-mill is 150r/min, and Ball-milling Time is 20h, and ball material mass ratio is 3: 1; Three, the mixture behind the ball milling is packed in rubber bag or the latex rubber bag, cold isostatic compaction obtains blank, and pressure is 22MPa, the porosity 40% of blank; Four, blank is put into the seal-off pressure container that is connected with recirculated water, then be filled with nitrogen and make the pressure in the seal-off pressure container reach 100MPa, igniting, the raw material self-propagating combustion namely prepares boron nitride-titanium carbonitride composite ceramic material.Other step and parameter are identical with embodiment 14.
Boron carbide powder in the present embodiment step 1, titanium valve all be purchase in market available.
Igniting in the present embodiment step 4 can be adopted the Ni-Cr resistance wire, and priming mixture has a variety of, simply can adopt granularity less than the mixture of the pure Ti powder of 300 orders and carbon black, and pure Ti powder and carbon black can be mixed by any ratio.
Self-propagating combustion in the present embodiment step 4 is recorded in the article of a piece " self-propagating combustion material synthesis technology " by name delivering on Zheng's bodyguard in 1999 " Shandong pottery " far away.
Present embodiment can be made large size, and (diameter is that 40～200mm, length are 50～1000mm) boron nitride-titanium carbonitride composite ceramic material.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, hundreds of times of room temperature-1000 ℃ cold cycling, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～150MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment 22: what present embodiment and embodiment 21 were different is to take by weighing 66% boron carbide powder, 34% titanium valve according to weight percent in the step 1.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 400 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～150MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment 23: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 63% boron carbide powder, 32% titanium valve and 5% boron nitride.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 600 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～140MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment 24: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 59% boron carbide powder, 34% titanium valve and 10% boron nitride.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～130MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 25: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 53% boron carbide powder, 17% titanium valve and 20% boron nitride.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～120MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 26: present embodiment and embodiment 21 are different, and to be boron nitride-titanium diboride ceramic composite material made by 46% boron carbide powder, 24% titanium valve and 30% Cr according to weight percent.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～110MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 27: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 40% boron carbide powder, 20% titanium valve and 40% TiC.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～100MPa, and bending strength can reach 50～80MPa under 2000 ℃ of hot conditionss.
Embodiment 28: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 33% boron carbide powder, 17% titanium valve and 50% TiC.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～100MPa, and bending strength can reach 50～70MPa under 2000 ℃ of hot conditionss.
Embodiment 29: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 26% boron carbide powder, 14% titanium valve and 60% TiC.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 400 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～140MPa, and bending strength can reach 50～70MPa under 2000 ℃ of hot conditionss.
Embodiment 30: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 75% boron carbide powder, 25% titanium valve.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 300 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～130MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Embodiment 31: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 50% boron carbide powder, 50% titanium valve.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～140MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Embodiment 32: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 20～80% boron carbide powder, 10%～70% titanium valve and 5～60% thinner powder.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～110MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 33: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 40% boron carbide powder, 20% titanium valve and 40% aluminium nitride.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～130MPa, and bending strength can reach 40～90MPa under 2000 ℃ of hot conditionss.
Embodiment 34: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 46% boron carbide powder, 24% titanium valve and 30% silicon carbide.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 400 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～140MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Embodiment 35: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 53% boron carbide powder, 17% titanium valve and 20% silicon oxide.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 600 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～150MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 36: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 40% boron carbide powder, 20% titanium valve and 40% silicon oxide.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～140MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Embodiment 37: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 33% boron carbide powder, 17% titanium valve and 50% silicon oxide.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 300 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 70～150MPa, and bending strength can reach 40～80MPa under 2000 ℃ of hot conditionss.
Embodiment 38: present embodiment and embodiment 21 are different be in the step 1 according to weight percent by 26% boron carbide powder, 14% titanium valve and 60% silicon oxide.Other step and parameter are identical with embodiment 21.
Present embodiment is made the boron nitride obtain-titanium carbonitride composite ceramic material can anti-high temperature more than 2600 ℃; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has extremely good heat-shock resistance, room temperature-1000 ℃ cold cycling 500 times, and product is without damage; The boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material has good processability, adopts different lathes all can process; The bending strength of the boron nitride that the present embodiment making obtains-titanium carbonitride composite ceramic material can reach 60～150MPa, and bending strength can reach 50～90MPa under 2000 ℃ of hot conditionss.
Claims (5)
1. the preparation method of boron nitride-titanium diboride ceramic composite material, it is characterized in that boron nitride-titanium diboride ceramic composite material makes according to following steps: one, raw material drying: take by weighing respectively 20%～80% boron carbide powder, 10%～70% titanium valve and 0%～70% thinner powder according to weight percent, and then the raw material that takes by weighing placed respectively under 80～150 ℃ the vacuum condition dry 8～12h; Two, raw material after the drying is put into ball mill and carried out the ball milling mixing, rotational speed of ball-mill is 100～200r/min, and Ball-milling Time is 12～24h, and ball material mass ratio is 3: 1; Three, the mixture behind the ball milling is packed in rubber bag or the latex rubber bag, cold isostatic compaction obtains blank, and pressure is 15～30MPa, the porosity 35%～45% of blank; Four, blank is put into the seal-off pressure container that is connected with recirculated water, then be filled with nitrogen and make the pressure in the seal-off pressure container reach 30～200MPa, igniting, the raw material self-propagating combustion namely prepares boron nitride-titanium carbonitride composite ceramic material.
2. the preparation method of boron nitride-titanium diboride ceramic composite material according to claim 1, it is characterized in that in the step 1 according to weight percent by 30%～60% boron carbide powder, 20%～50% titanium valve and 0%～60% thinner powder, and each component content sum is 100%.
3. the preparation method of boron nitride-titanium diboride ceramic composite material according to claim 1 and 2 is characterized in that the thinner powder is ceramic-like thinner powder and/or metal species thinner powder.
4. the preparation method of boron nitride-titanium diboride ceramic composite material according to claim 3 is characterized in that ceramic-like thinner powder is by BN, AlN, SiC, HfC, ZrC, TiC, Si
3N
4, MoSi
2, Al
2O
3, ZrO
2, CaO, MgO, SiO
2, Y
2O
3, aluminium titanates, mullite and TiO
2In a kind of or several compositions wherein.
5. the preparation method of boron nitride-titanium diboride ceramic composite material according to claim 3 is characterized in that metal species thinner powder is by a kind of among Ni, W, Cr, Co, Fe, Cu, V, Pd, Ir, Rh, Re, Os, Ru, Hf and the Ta or several composition the wherein.
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| CN103952650B (en) * | 2014-04-23 | 2016-03-02 | 山东大学 | Boron nitride nano-tube strengthens the preparation method of titanium carbide nitride based metal ceramic cutter material |
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