CN1266078C - SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof - Google Patents
SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof Download PDFInfo
- Publication number
- CN1266078C CN1266078C CN 200410044158 CN200410044158A CN1266078C CN 1266078 C CN1266078 C CN 1266078C CN 200410044158 CN200410044158 CN 200410044158 CN 200410044158 A CN200410044158 A CN 200410044158A CN 1266078 C CN1266078 C CN 1266078C
- Authority
- CN
- China
- Prior art keywords
- powder
- silicone oil
- containing hydrogen
- hydrogen silicone
- pottery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Ceramic Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a Si-Al-O-N-C ceramic prepared from hydrogenous silicon oil and Al powder and a preparation method thereof, which relates to a ceramic prepared from organic polymers and active components thereof and a preparation method thereof. The ceramic has the components by weight percentage of 18 to 55% of hydrogenous silicon oil, 43% to 70% of amino compound and 2 to 22% of Al powder. In the preparation method, according to the weight percentage, 18 to 55% of the hydrogenous silicon oil, 43% to 70% of the amino compound, 2 to 22% of the Al powder are taken to be mixed and stirred at the temperature from 0 to 100 DEG C for 8 to 12 hours, and through reaction, the Si-Al-O-N-C organic polymer is produced; the organic polymer is put in a hot-pressing sintering furnace, nitrogen of 0.5 to 1 atm is led in, the pressured is increased by 15 to 20MPa, or nitrogen of 5 to 12 atm is led in a gas pressure sintering furnace, the sintering temperature is from 1600 to 1750 DEG C, the temperature is preserved for 1 to 2 hours, and the Si-Al-O-N-C ceramic is sintered. The Si-Al-O-N-C ceramic of the present invention has the advantages of high specific strength, low production cost, etc.
Description
Technical field:
The present invention relates to a kind of pottery of using organic polymer and active constituent preparation thereof and preparation method thereof, be specifically related to a kind of Si-Al-O-N-C pottery of using containing hydrogen silicone oil and the preparation of Al powder and preparation method thereof.
Background technology:
In high-temperature material fields such as machinery, aerospace, the energy and military affairs, the requirement at aspects such as specific tenacity, specific rigidity, hardness, toughness, wear resisting property, corrosion resistance nature and high-temperature behaviors grows with each passing day to material.Because metallic substance is subjected to the restriction of use temperature and autologous density, normal SiC, the Si of using in these fields
3N
4, high temperature structural ceramics and matrix material thereof such as Sialon, but these potteries but can only can not use because of its high volatile volatile in the combustion gas environment between 1300～1400 ℃ steady in a long-term use the below 1200～1300 ℃.In addition, also there is the defective of using as structural part in the inside of these materials, and material is more crisp, be unfavorable for processing, and reliability of material can be poor, and relative cost is higher; Use organic polymer to have as the material of preparation pottery that firing temperature is low, purity is high, thermoplasticity is good, advantages such as easy dissolving, easy machine-shaping, pottery with this material making, its preparation method has many-sided application, can be processed into fiber, film, crosslinking curing becomes complex shaped components etc.In addition, with the stupalith of organic polymer preparation based on unformed non-crystalline state, these materials generally have excellent high temperature oxidation resistance, but there is the raw materials cost height in the pottery that utilizes this material preparation, complicated process of preparation, problems such as ceramic yield is low, thus limited applying of it.
Summary of the invention:
It is low to the purpose of this invention is to provide a kind of production cost, simple, the operation easily of preparation method, and the production efficiency height is used Si-Al-O-N-C pottery of containing hydrogen silicone oil and Al powder preparation and preparation method thereof.The raw material of the Si-Al-O-N-C pottery with the preparation of containing hydrogen silicone oil and Al powder of the present invention is made up of according to weight percent following component: containing hydrogen silicone oil 18～55%, amino-complex 43%～70%, Al powder 2～22%.Preparation method of the present invention may further comprise the steps: a, get containing hydrogen silicone oil 18～55%, amino-complex 43～70%, Al powder 2～22% by weight percentage and mix, be constantly to stir 8～12 hours under 0～100 ℃ the condition in temperature, reaction forms the Si-Al-O-N-C organic polymer; B, the product that previous step is obtained in rapid are contained in hot pressing or the gas pressure sintering stove, feed nitrogen, in hot-pressed sintering furnace, feed 0.5～1 the atmospheric nitrogen and the 15～20MPa that pressurizes, or in the gas pressure sintering stove, feed 5～12 atmospheric nitrogen, sintering temperature is controlled between 1600～1750 ℃, be incubated 1～2 hour, obtain fine and close Si-Al-O-N-C pottery behind the sintering.
The present invention has following beneficial effect: 1, the present invention adopts the main raw material of cheap organic containing hydrogen silicone oil as the preceramic organosilicon polymer body, with Al part as active constituent, from reducing the cost of preceramic organosilicon polymer body, simplifying aspects such as preparation technology and raising ceramic green productive rate considers, organic silicone oil is applied to prepare stupalith in the Si-Al-O-N-C system, can improves specific tenacity, specific rigidity, hardness, toughness and wear-resisting, high temperature resistant, the corrosion resistance nature of material.2, containing hydrogen silicone oil, diethylenetriamine and the mixing of Al powder, reaction are formed with organic polymer, and organic polymer is sintered directly into pottery, based on non-crystalline state, density is 2.0～2.5g/cm to this pottery between 1000～1750 ℃
3, bending strength is 50～250Mpa, fracture toughness property is 1.9～4.0MPam
1/2, Vickers' hardness is 0.6～7.4Gpa, the output capacity of pottery reaches 90～93%.3, containing hydrogen silicone oil, quadrol and the mixing of Al powder, reaction are formed with organic polymer, and organic polymer is sintered directly into pottery, based on non-crystalline state, density is 2.0～2.5g/cm to this pottery between 1000～1750 ℃
3, bending strength is 50～300Mpa, fracture toughness property is 1.9～3.4Mam
1/2, Vickers' hardness is 0.6～6.0Gpa, the output capacity of pottery reaches 78～94%.4, preparation method of the present invention is simple, operation easily, and ceramic output capacity height, the thermal stability of the stupalith that obtains is good.5, the Si-Al-O-N-C stupalith with containing hydrogen silicone oil and the preparation of Al powder of the present invention can be widely used in high-temperature material fields such as machinery, aerospace, the energy and military affairs.
Embodiment:
Embodiment one: the raw material with the Si-Al-O-N-C pottery of containing hydrogen silicone oil and Al powder preparation of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 18～55%, amino-complex 43%～70%, Al powder 2～22%, described amino-complex are diethylenetriamine or quadrol.
Embodiment two: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 18～37%, diethylenetriamine 50～70%, Al powder 3～22%.
Embodiment three: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 18%, diethylenetriamine 70%, Al powder 12%.
Embodiment four: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 37%, diethylenetriamine 60%, Al powder 3%.
Embodiment five: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 28%, diethylenetriamine 50%, Al powder 22%.
Embodiment six: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 37～55%, quadrol 43～60%, Al powder 2～10%.
Embodiment seven: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 37%, quadrol 60%, Al powder 3%.
Embodiment eight: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 40%, quadrol 50%, Al powder 10%.
Embodiment nine: the raw material of the Si-Al-O-N-C pottery of present embodiment is made up of according to weight percent following component: containing hydrogen silicone oil 55%, quadrol 43%, Al powder 2%.
Embodiment ten: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, get containing hydrogen silicone oil 18～55%, amino-complex 43～70%, Al powder 2～22% by weight percentage and mix, be constantly to stir 8～12 hours under 0～100 ℃ the condition in temperature, reaction forms the Si-Al-O-N-C organic polymer; B, the product that previous step is obtained in rapid are contained in hot pressing or the gas pressure sintering stove, feed nitrogen, in hot-pressed sintering furnace, feed 0.5～1 the atmospheric nitrogen and the 20MPa that pressurizes, or in the gas pressure sintering stove, feed 5～12 atmospheric nitrogen, sintering temperature is controlled between 1600～1750 ℃, be incubated 1～2 hour, obtain fine and close Si-Al-O-N-C pottery behind the sintering, described amino-complex is diethylenetriamine or quadrol.
Embodiment 11: the difference of present embodiment and embodiment ten is; it also increases a ' step between a, b step: the product that previous step is obtained in rapid is contained in the tubular type atmosphere protection stove; in temperature is that the feeding flow is the nitrogen of 200～400ml/min between 200～1000 ℃; heat-up rate is controlled at 0.1～10 ℃/min; reacted 8～12 hours; the Si-Al-O-N-C organic polymer is carried out cracking, obtain the Si-Al-O-N-C powder.
Embodiment 12: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 169ml, diethylenetriamine 270ml and Al powder 15 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 37%, diethylenetriamine 60% and Al powder 3%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow between room temperature～750 ℃ is the nitrogen of 200～400ml/min, heat-up rate is 5 ℃/min, insulation is 1 hour when temperature reaches 750 ℃, in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, and insulation is 1 hour when temperature reaches 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the hot-pressed sintering furnace, feeds 1 the atmospheric nitrogen and the 20MPa that pressurizes in hot-pressed sintering furnace, the control sintering temperature is 1750 ℃, be incubated 1 hour, obtains the Si-Al-O-N-C pottery of densification behind the sintering.
The pottery output capacity is 90%, and density is 2.5g/cm
3, bending strength is 231MPa, fracture toughness property is 4.0MPam
1/2, Vickers' hardness is 7.4Gpa.
Embodiment 13: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 40ml, diethylenetriamine 140ml and Al powder 49 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-Q-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 18%, diethylenetriamine 60% and Al powder 22%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the hot-pressed sintering furnace, feeds 1 the atmospheric nitrogen and the 20MPa that pressurizes in hot-pressed sintering furnace, 1750 ℃ of control sintering temperatures be incubateds 1 hour, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
The pottery output capacity is 93.9%, and density is 1.9g/cm
3, bending strength is 47MPa, fracture toughness property is 1.9MPam
1/2, Vickers' hardness is 0.6Gpa.
Embodiment 14: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 169ml, diethylenetriamine 270ml and Al powder 15 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 37%, diethylenetriamine 60% and Al powder 3%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the gas pressure sintering stove, feeding pressure is the nitrogen of 1.2MPa, and the control sintering temperature be incubated 1 hour between 1600～1750 ℃, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
Embodiment 15: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 40ml, diethylenetriamine 140ml and Al powder 49 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 18%, diethylenetriamine 60% and Al powder 22%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the gas pressure sintering stove, feeding pressure is the nitrogen of 1.2MPa, and the control sintering temperature be incubated 1 hour between 1600～1750 ℃, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
Embodiment 16: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 68ml, quadrol 70ml and Al powder 15 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 45%, quadrol 45% and Al powder 10%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the hot-pressed sintering furnace, feeds 1 the atmospheric nitrogen and the 15MPa that pressurizes in hot-pressed sintering furnace, the control sintering temperature is 1600 ℃, be incubated 1 hour, obtains the Si-Al-O-N-C pottery of densification behind the sintering.
The pottery output capacity is 93.6%, and density is 2.0g/cm
3, bending strength is 37MPa, fracture toughness property is 1.0MPam
1/2, Vickers' hardness is 0.6Gpa.
Embodiment 17: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 169ml, quadrol 274ml and Al powder 15 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 37%, quadrol 60% and Al powder 3%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the hot-pressed sintering furnace, feeds 1 the atmospheric nitrogen and the 15MPa that pressurizes in hot-pressed sintering furnace, the control sintering temperature is 1600 ℃, be incubated 1 hour, obtains the Si-Al-O-N-C pottery of densification behind the sintering.
The pottery output capacity is 92.5%, and density is 2.4g/cm
3, bending strength is 252MPa, fracture toughness property is 3.2MPam
1/2Vickers' hardness is 6.1Gpa.
Embodiment 18: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 198ml, quadrol 155ml and Al powder 6 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 55%, quadrol 43% and Al powder 2%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the hot-pressed sintering furnace, feeds 1 the atmospheric nitrogen and the 15MPa that pressurizes in hot-pressed sintering furnace, the control sintering temperature is 1600 ℃, be incubated 1 hour, obtains the Si-Al-O-N-C pottery of densification behind the sintering.
The pottery output capacity is 81.5%, and density is 2.5g/cm
3, bending strength is 267MPa, fracture toughness property is 3.3MPam
1/2, Vickers' hardness is 5.3Gpa.
Embodiment 19: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 104ml, quadrol 102ml and Al powder 5 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 49%, quadrol 49% and Al powder 2%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the hot-pressed sintering furnace, feeds 1 the atmospheric nitrogen and the 15MPa that pressurizes in hot-pressed sintering furnace, the control sintering temperature is 1600 ℃, be incubated 1 hour, obtains the Si-Al-O-N-C pottery of densification behind the sintering.
The pottery output capacity is 76.8%, and density is 2.3g/cm
3, bending strength is 230MPa, fracture toughness property is 2.6MPam
1/2, Vickers' hardness is 5.0Gpa.
Embodiment 20: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 68ml, quadrol 70ml and Al powder 15 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 45%, quadrol 45% and Al powder 10%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the gas pressure sintering stove, feeding pressure is the nitrogen of 1.2MPa, and the control sintering temperature be incubated 1 hour between 1600～1750 ℃, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
Embodiment 21: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 169ml, quadrol 274ml and Al powder 15 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 37%, quadrol 60% and Al powder 3%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the gas pressure sintering stove, feeding pressure is the nitrogen of 1.2MPa, and the control sintering temperature be incubated 1 hour between 1600～1750 ℃, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
Embodiment 22: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 198ml, quadrol 155ml and Al powder 6 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 55%, quadrol 43% and Al powder 2%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the gas pressure sintering stove, feeding pressure is the nitrogen of 1.2MPa, and the control sintering temperature be incubated 1 hour between 1600～1750 ℃, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
Concrete implement 23: present embodiment prepare the preparation method of Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, its preparation process is: a, containing hydrogen silicone oil 104ml, quadrol 102ml and Al powder 5 grams are mixed, use tetrahydrofuran (THF) 500ml and normal hexane 250ml as solvent, constantly stirred at normal temperatures 8～12 hours, reaction forms the Si-Al-O-N-C organic polymer, and the weight percent in the Si-Al-O-N-C organic polymer raw material is: containing hydrogen silicone oil 49%, quadrol 49% and Al powder 2%; B, the Si-Al-O-N-C organic polymer is contained in the tubular type atmosphere protection stove Si-Al-O-N-C organic polymer is carried out cracking, feeding flow is the nitrogen of 200～400ml/min, temperature is between room temperature～750 ℃, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 750 ℃, and in 750～1000 ℃ temperature range, heat-up rate is 5 ℃/min, insulation is 1 hour in the time of 1000 ℃, obtains the Si-Al-O-N-C powder; C, prepared Si-Al-O-N-C powder is contained in the gas pressure sintering stove, feeding pressure is the nitrogen of 1.2MPa, and the control sintering temperature be incubated 1 hour between 1600～1750 ℃, obtain the Si-Al-O-N-C pottery of densification behind the sintering.
Claims (9)
1, a kind of Si-A1-O-N-C pottery with containing hydrogen silicone oil and the preparation of Al powder is characterized in that its raw material is made up of according to weight percent following component: containing hydrogen silicone oil 18～55%, amino-complex 43%70%, Al powder 2～22%; The preparation method of described Si-Al-O-N-C pottery may further comprise the steps: a, get containing hydrogen silicone oil 18～55%, amino-complex 43～70%, Al powder 2～22% by weight percentage and mix, be constantly to stir 8～12 hours under 0～100 ℃ the condition in temperature, reaction forms the Si-Al-O-N-C organic polymer; B, the product that previous step is obtained in rapid are contained in hot pressing or the gas pressure sintering stove, feed nitrogen, in hot-pressed sintering furnace, feed 0.5～1 the atmospheric nitrogen and the 15～20MPa that pressurizes, or in the gas pressure sintering stove, feed 5～12 atmospheric nitrogen, sintering temperature is controlled between 1600～1750 ℃, be incubated 1～2 hour, obtain fine and close Si-Al-O-N-C pottery behind the sintering.
2, the Si-Al-O-N-C pottery with containing hydrogen silicone oil and the preparation of Al powder according to claim 1 is characterized in that amino-complex is diethylenetriamine or quadrol.
3, the Si-Al-O-N-C pottery with containing hydrogen silicone oil and the preparation of Al powder according to claim 1 and 2 is characterized in that its raw material is made up of according to weight percent following component: containing hydrogen silicone oil 18～37%, diethylenetriamine 50～70%, Al powder 3～22%.
4, the Si-Al-O-N-C pottery with containing hydrogen silicone oil and the preparation of Al powder according to claim 3 is characterized in that its raw material is made up of according to weight percent following component: containing hydrogen silicone oil 37%, diethylenetriamine 60%, Al powder 3%.
5, the Si-Al-O-N-C pottery with containing hydrogen silicone oil and the preparation of Al powder according to claim 1 and 2 is characterized in that its raw material is made up of according to weight percent following component: containing hydrogen silicone oil 37～55%, quadrol 43～60%, Al powder 2～10%.
6, the Si-Al-O-N-C pottery with containing hydrogen silicone oil and the preparation of Al powder according to claim 5 is characterized in that its raw material is made up of according to weight percent following component: containing hydrogen silicone oil 55%, quadrol 43%, Al powder 2%.
7, the preparation method who prepares the Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder, it is characterized in that it may further comprise the steps: a, get containing hydrogen silicone oil 18～55%, amino-complex 43～70%, Al powder 2～22% by weight percentage and mix, be constantly to stir 8～12 hours under 0～100 ℃ the condition in temperature, reaction forms the Si-Al-O-N-C organic polymer; B, the product that previous step is obtained in rapid are contained in hot pressing or the gas pressure sintering stove, feed nitrogen, in hot-pressed sintering furnace, feed 0.5～1 the atmospheric nitrogen and the 15～20MPa that pressurizes, or in the gas pressure sintering stove, feed 5～12 atmospheric nitrogen, sintering temperature is controlled between 1600～1750 ℃, be incubated 1～2 hour, obtain fine and close Si-Al-O-N-C pottery behind the sintering.
8, the preparation method who prepares the Si-Al-O-N-C pottery with containing hydrogen silicone oil and Al powder according to claim 7; it is characterized in that also comprising a ' step between a, b step: the product that previous step is obtained in rapid is contained in the tubular type atmosphere protection stove; in temperature is that the feeding flow is the nitrogen of 200～400ml/min between 200～1000 ℃; temperature rise rate is controlled at 0.1～10 ℃/min; reacted 8～12 hours; the Si-Al-O-N-C organic polymer is carried out cracking, obtain the Si-Al-O-N-C powder.
9, according to claim 7ly prepare the preparation method of Si-Al-O-N-C pottery, it is characterized in that amino-complex is diethylenetriamine or quadrol with containing hydrogen silicone oil and Al powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410044158 CN1266078C (en) | 2004-12-22 | 2004-12-22 | SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410044158 CN1266078C (en) | 2004-12-22 | 2004-12-22 | SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1644564A CN1644564A (en) | 2005-07-27 |
| CN1266078C true CN1266078C (en) | 2006-07-26 |
Family
ID=34868651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410044158 Expired - Fee Related CN1266078C (en) | 2004-12-22 | 2004-12-22 | SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1266078C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439288C (en) * | 2006-12-14 | 2008-12-03 | 哈尔滨工业大学（威海） | Sialon quasi monodimension nanometer material and its preparation method |
| CN101857437B (en) * | 2010-06-30 | 2012-08-22 | 中国人民解放军国防科学技术大学 | Si-Al-O-C ceramic material and preparation method thereof |
| CN106582116B (en) * | 2017-01-12 | 2019-04-26 | 哈尔滨工业大学（威海） | A kind of preparation method and device of medicine intermediate filtering material |
-
2004
- 2004-12-22 CN CN 200410044158 patent/CN1266078C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1644564A (en) | 2005-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Flores et al. | Ceramic fibers based on SiC and SiCN systems: current research, development, and commercial status | |
| US8778488B2 (en) | Formation of silicon carbide-silicon nitride nanoparticle carbon compositions | |
| CN101240070B (en) | Method for synthesizing supercritical fluid of ceramic precursor polycarbosilane | |
| CN108129151B (en) | Graphene/silicon carbide nano composite structure monolithic ceramic and preparation method thereof | |
| CN101033137A (en) | Method of preparing carbon/carbon-silicon carbide ceramics base composite material | |
| CN108675772B (en) | Preparation method of alumina/graphene core-shell structure composite material | |
| CN1793042A (en) | In-situ flexible silicon nitride base ceramic and super-speed sintering process | |
| JP2013500226A (en) | High toughness ceramic composite material | |
| CN113121242A (en) | Short carbon fiber toughened silicon carbide composite material and preparation method thereof | |
| CN111517797B (en) | Low-temperature normal-pressure sintering preparation method of high-purity SiC ceramic coating capable of being produced in mass | |
| CN1266078C (en) | SiALONC ceramic with hydrogen silicone oil and Al powder and production thereof | |
| CN105669982B (en) | A kind of organometallic polymer complex phase ceramic precursor and the preparation method and application thereof | |
| KR101101244B1 (en) | Method for manufacturing high density SiCf/SiC composites | |
| CN1727307A (en) | Ceramics of silicon nitride with high antioxygenic property and preparation method | |
| EP2716617A1 (en) | Method for producing silicon carbide-carbon composite | |
| CN112500574B (en) | Ti-containing Si-C-N ceramic precursor and synthesis method and application thereof | |
| CN1654430A (en) | Low temperature sintering method for high hardness silicon nitride ceramics | |
| CN110105070B (en) | Continuous silicon carbide fiber with controllable electrical property and wide range and preparation method thereof | |
| CN100404465C (en) | Method for preparing TiN/Al2O3 composite materials | |
| US7112547B2 (en) | Highly heat-resistant inorganic fiber-bonded ceramic component and process for the production thereof | |
| CN101054297A (en) | Method for preparing nano polyphase ceramic powder | |
| CN1272244C (en) | B6O nanowire and crystal whisker structure and its preparation method | |
| CN1597619A (en) | Preparation method of whisker and pacticle toughening ceramic base composite | |
| CN1637159A (en) | In-situ hot pressing process of synthesizing compact composite carbon titanosilicide-titanium diboride bulk material | |
| JP3969106B2 (en) | High heat resistant inorganic fiber bonded ceramic bonded body and bonding method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |