CN102826852A - Preparation method of titanium nitride-alumina complex phase wear resistant high-temperature resistant ceramics material - Google Patents
Preparation method of titanium nitride-alumina complex phase wear resistant high-temperature resistant ceramics material Download PDFInfo
- Publication number
- CN102826852A CN102826852A CN2012103188954A CN201210318895A CN102826852A CN 102826852 A CN102826852 A CN 102826852A CN 2012103188954 A CN2012103188954 A CN 2012103188954A CN 201210318895 A CN201210318895 A CN 201210318895A CN 102826852 A CN102826852 A CN 102826852A
- Authority
- CN
- China
- Prior art keywords
- content
- titanium nitride
- preparation
- resistant
- alumina
- 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.)
- Granted
Links
Landscapes
- Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明涉及一种氮化钛-氧化铝复相耐磨耐高温陶瓷材料的制备方法，属于耐磨耐高温材料技术领域。其特征是以工业固体废弃物铝灰、金红石矿粉或金红石型钛白粉为主要原料，以铝灰中的金属铝为还原剂，采用铝热还原氮化工艺制备了氮化钛-氧化铝复合粉体，再利用得到的复相粉体制备氮化钛-氧化铝复相耐磨耐高温陶瓷，实现废铝灰的循环再利用和环境保护。所述氮化钛-氧化铝复相耐磨耐高温陶瓷材料的制备方法具有工艺流程简单，环境污染小，制造成本较低等诸多优势，具有广泛的社会和经济价值。The invention relates to a preparation method of a titanium nitride-alumina composite phase wear-resistant and high-temperature resistant ceramic material, belonging to the technical field of wear-resistant and high-temperature resistant materials. It is characterized by using industrial solid waste aluminum ash, rutile ore powder or rutile titanium dioxide as the main raw material, using metal aluminum in the aluminum ash as the reducing agent, and using the aluminothermic reduction nitriding process to prepare titanium nitride-alumina composite powder, and then use the obtained composite powder to prepare titanium nitride-alumina composite phase wear-resistant and high-temperature ceramics, so as to realize the recycling and environmental protection of waste aluminum ash. The preparation method of the titanium nitride-alumina composite phase wear-resistant and high-temperature resistant ceramic material has many advantages such as simple process flow, less environmental pollution, and lower manufacturing cost, and has extensive social and economic value.
Description
Technical field
The present invention relates to a kind of preparation method of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material, belong to Wear-resistant, high-temperature resistant material technology field.
Background technology
Erosive wear is one of principal mode of material damage, accounts for 8% of the sum of wear-out failure in the industrial production, and it is meant that fluid or solids impact the wearing and tearing that caused with loose small-particle according to certain speed and angle to material surface.In industry, the Dual-Phrase Distribution of Gas olid erosive wear phenomenon under the high temperature exists particularly general, and harm is bigger.At present, mainly adopt heat-resisting alloy steel, alumina-ceramic and zirconia ceramics both at home and abroad in this respect.The former ubiquity is high temperature resistant abrasion poor-performing, cost an arm and a leg, high temperature (above 1000 ℃) is prone to weakness such as softening, thereby causes defectives such as its wear resisting property is relatively poor, work-ing life is short; The latter can satisfy resistant to elevated temperatures requirement, but exists that fragility is big, heat-resistant stable property is not good enough and shortcoming such as poor toughness, is prone to cause problems such as bulk is peeled off, work-ing life is short thereby cause under hot environment, working.Research shows, through adding the second phase particle, can improve the toughness and the high temperature resistant erosive wear performance of ceramic matrix material, prepares novel high temperature resistant Dual-Phrase Distribution of Gas olid erosive wear protective material.
TiN-Al
2O
3Diphase ceramic material is a kind of non-oxide ceramic material of excellent performance, at Al
2O
3Introduce TiN in the matrix, utilize its advantage separately, not only can improve its intensity, toughness and wear resistance, be used to make the high-temperature wearable structure unit.TiN and Al
2O
3Complex method a lot, comprise Al
2O
3With TiN powder mechanically mixing, TiO
2-Al
2O
3Composite granule is at mobile NH
3Nitride selectivity under the atmosphere, be that reductive agent is at N with the aluminium powder
2Under the atmosphere with TiO
2Thermite reduction nitrogenize etc.Wherein, traditional mechanically mixing mode is prone to cause the reunion of adding phase or cause local component deviation, influences composite property; Utilize NH
3The method of atmosphere nitride selectivity has greater environmental impacts; Utilizing aluminium powder to carry out the thermite reduction nitrogenizing reaction then can make manufacturing cost improve because of the higher meeting of aluminium powder price.
Rutile is a kind of important raw mineral materials that refines titanium; It has excellent properties such as high temperature resistant, low temperature resistant, corrosion-resistant, HS; Be widely used in aspects such as aerospace, machinery, chemical industry, sea water desaltination, rutile is still produced the important source material of Rutile type Titanium Dioxide and high-grade welding electrode in addition.Utilize rutile or the relevant normal method such as nitridation in situ or aluminothermy nitrogenize under carbon nitrogenize, the ammonia atmosphere of burying that adopts of feedstock production titanium nitride that contains titanium oxide.
The aluminium ash is the solid waste that the slag that produces in electrolytic aluminum, the processes such as casting aluminium etc. and outer skin discharge after processing, and it mainly comprises Al, Al
2O
3, AlN, MgO and SiO
2Etc. chemical ingredients, also have some muriates and sulfide etc., the ratio of its chemical ingredients is along with the raw material and the operational condition of each manufacturer are different and slightly different.The aluminium ash is big, the with serious pollution industrial residue of a kind of output, and according to statistics, every production 1000t aluminium will produce 25t left and right sides aluminium ash.The aluminium ash is used as rubbish usually and abandons, not only contaminate environment, but also need to dispose the place in a large number, and processing costs is high.Along with the development of industrial process, the turnout of aluminium ash is more and more, and how fully utilizing the aluminium ash is a worldwide important topic.The aluminium ash is a kind of solid waste; Also be a kind of renewable resources simultaneously; According to domestic and foreign literature; The aluminium ash has obtained application with covering slag, furnace refractory, concrete and road with fields such as materials at composition, electric-arc furnace steelmakings such as reclaiming metallic aluminium, salt, aluminum oxide, but present several kinds utilize approach to have complex technical process, produce secondary pollution, consume mass energy, the grey consumption of aluminium is little, these a large amount of aluminium ashes for continuous generation still produce little effect.Therefore, propose, and the thinking that is used to produce high demand material is a kind of effective way of dealing with problems, for example the aluminium ash is converted into the starting material of refractory materials industrial solid waste residue resources such as aluminium ashes.Adopt aluminium ash production refractory materials, report main fused brown corundum or the magnesium aluminate spinel compoud etc. of producing at present, but because of containing Al in these production processes requirement aluminium ashes
2O
3High and not exclusively there is limitation in the utilization of aluminium ash component.
Therefore; The present invention is on the basis of the newest research results of titanium nitride-alumina composite diphase material; By environmental protection, save energy, the technological thought that reduces cost; Novelty ground is raw material with industrial solid castoff aluminium ash and rutile breeze or Rutile type Titanium Dioxide; Prepared titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material through thermite reduction nitrogenizing reaction, pressureless sintering method,, the wide industrial applying value has been arranged as a kind of novel high temperature resistant Dual-Phrase Distribution of Gas olid erosive wear protective material.
Summary of the invention
Patented claim of the present invention is to prepare in the technological process of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material at industrial solid castoff aluminium ash and Rutile type Titanium Dioxide or rutile breeze thermite reduction nitrogenizing reaction, pressureless sintering method; Through controlling aluminium ash amount of allocating into and thermite reduction nitrogenizing reaction temperature with the control reaction process; Through the temperature and the soaking time of control pressureless sintering, realize the preparation of titanium nitride-alumina multi-phase wear-resistant high temperature material.The present invention has that technical process is simple, cost is lower, turns waste into wealth, many advantages such as environmental pollution is little, added value of product height, to the production cost that reduces the titanium nitride-alumina complex phase ceramic, promote the cyclic utilization rate of solid waste such as aluminium ash and reduce environmental pollution etc. and be of great practical significance and social value.
The preparation method of a kind of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the present invention proposes; It is characterized in that: in total batching quality
aluminium ash; And
rutile breeze or Rutile type Titanium Dioxide are raw material; Prepare the sample green compact through technological processs such as batching, ball milling, moulding; Adopt the thermite reduction nitriding 1100 ℃～1500 ℃, insulation 0.1 hour～100 hours, prepare the titanium nitride-alumina composite powder material.Then the powder body material that obtains is handled through dry-pressing formed, isostatic cool pressing and obtained ceramic body; Under nitrogen atmosphere, adopt pressureless sintering method 1400 ℃～1800 ℃, insulation 0.1 hour～100 hours, obtain titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material behind the naturally cooling.Wherein dry-pressing formed pressure is 0.1～60MPa, and the pressure action time is 10～60s; The pressure that isostatic cool pressing is handled is 150～300MPa, and the pressure action time is 60～120s.
The preparation method of a kind of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the present invention proposes, described technical process is specially:
1) with raw materials such as aluminium ash, rutile breeze or Rutile type Titanium Dioxides through processing such as pulverizing, grind and sieve, make its particle diameter respectively less than 200 μ m and 100 μ m.Then by both certainty ratios batching and its thorough mixing is even, more mixed raw material is packed in the ball grinder, adopt dry ball milling ball milling 0.1～50 hour to each raw material in planetary ball mill to be uniformly dispersed; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing 10～60s of the condition of 0.1～60MPa, process columned sample green compact.
2) with the above-mentioned green compact that prepare put into can be anti-the high-temperature resistant container (like plumbago crucible) of temperature more than 1800 ℃; Put it in atmosphere furnace, electric arc furnace or the induction furnace of nitrogen atmosphere; Heat-up rate is 1～10 ℃/min; After insulation
under 1100 ℃～1500 ℃; Take out after naturally cooling to room temperature, can obtain particle diameter titanium nitride-alumina composite powder material comparatively uniformly through processing such as pulverizing, grind, sieve.
3) adopt dry pressing that above-mentioned powder body material is acted on 10～60s under the condition of 0.1～60MPa; Obtain having the base substrate of certain its density; Under 150～300MPa, carry out isostatic cool pressing then and handle 60～120s, obtain the titanium nitride-alumina ceramic green.Subsequently; With green compact put into can be anti-the high-temperature resistant container (like plumbago crucible) of temperature more than 1800 ℃; Put it in atmosphere furnace, electric arc furnace or the induction furnace of nitrogen atmosphere protection; Heat-up rate is 1～10 ℃/min, after naturally cooling to room temperature after the insulation
under 1400 ℃～1800 ℃, can obtain titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
The present invention has realized the preparation purpose of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material through effectively controlling the temperature and the reaction process of thermite reduction nitrogenizing reaction under better simply technical process.This production process has many advantages such as environmental pollution is little, cost is lower, added value of product height, to the production cost that reduces the titanium nitride-alumina complex phase ceramic, promote the cyclic utilization rate of solid waste such as aluminium ash and reduce aspect such as environmental pollution and be of great practical significance and social value.
Embodiment
Below in conjunction with instance technical scheme of the present invention is further specified, but is not only to be confined to following embodiment:
Embodiment 1
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of rutile breeze and granularity requirements are: TiO
2Content is 99.20wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully, take by weighing raw material respectively, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed according to weight percent aluminium scrap ash 63%, rutile breeze 37%; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1100 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1600 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 1 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 588.2MPa, the fracture toughness property value is 5.18MPam
1/2
Embodiment 2
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of rutile breeze and granularity requirements are: TiO
2Content is 99.20wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully, take by weighing raw material respectively, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed according to weight percent aluminium scrap ash 57%, rutile breeze 43%; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1200 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1600 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 2 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 588.2MPa, the fracture toughness property value is 5.18MPam
1/2
Embodiment 3
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of rutile breeze and granularity requirements are: TiO
2Content is 99.20wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully, take by weighing raw material respectively, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed according to weight percent aluminium scrap ash 67%, rutile breeze 33%; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1300 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1600 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 3 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 588.2MPa, the fracture toughness property value is 5.18MPamm
1/2
Embodiment 4
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of rutile breeze and granularity requirements are: TiO
2Content is 99.20wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully, take by weighing raw material respectively, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed according to weight percent aluminium scrap ash 72%, rutile breeze 28%; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1400 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1600 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 4 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 588.2MPa, the fracture toughness property value is 5.18MPam
1/2
Embodiment 5
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of Rutile type Titanium Dioxide and granularity requirements are: TiO
2Content is 99.80wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully; Take by weighing raw material respectively according to weight percent aluminium scrap ash 63%, Rutile type Titanium Dioxide 37%, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1100 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1500 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 5 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 593.1MPa, the fracture toughness property value is 5.27MPam
1/2
Embodiment 6
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of Rutile type Titanium Dioxide and granularity requirements are: TiO
2Content is 99.80wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully; Take by weighing raw material respectively according to weight percent aluminium scrap ash 57%, Rutile type Titanium Dioxide 43%, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1200 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1500 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 6 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 593.1MPa, the fracture toughness property value is 5.27MPam
1/2
Embodiment 7
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of Rutile type Titanium Dioxide and granularity requirements are: TiO
2Content is 99.80wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully; Take by weighing raw material respectively according to weight percent aluminium scrap ash 67%, Rutile type Titanium Dioxide 33%; Adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm, and place the nitrogen atmosphere stove, under flowing nitrogen atmosphere with heat-up rate be 5 ℃/min be warming up to 1300 ℃ the insulation 5 hours; Take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1500 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 7 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 593.1MPa, the fracture toughness property value is 5.27MPam
1/2
Embodiment 8
The staple and the granularity requirements of industrial solid castoff aluminium ash raw material are: Al content is 26.5wt.%, Al
2O
3Content is that 6.23wt.%, AlN content are 16.69wt.%, MgAl
2O
4Content is 22.17wt.%, SiO
2Content is that 5.16wt.%, NaCl content are that 4.32wt.%, CaO content are 2.36wt.%, TiO
2Content is 5.75wt.%, Fe
2O
3Content is 3.49wt.%, and its particle diameter is less than 200 μ m.The staple of Rutile type Titanium Dioxide and granularity requirements are: TiO
2Content is 99.80wt.%, and its particle diameter is less than 100 μ m.
According to TiO
2Be the theoretical consumption that TiN calculates required aluminium ash by the aluminium reducing in the aluminium ash fully; Take by weighing raw material respectively according to weight percent aluminium scrap ash 72%, Rutile type Titanium Dioxide 28%, adopt dry ball milling ball milling 10 hours to each raw material in planetary ball mill to be uniformly dispersed; Then with the uniform raw material of ball mill mixing at the dry-pressing formed processing of the condition of 20MPa 15s; Process the sample green compact of Φ 20mm * 20mm; And place the nitrogen atmosphere stove; Under flowing nitrogen atmosphere, be that 5 ℃/min is warming up to 1400 ℃ of insulations 5 hours, take out after naturally cooling to room temperature with stove, obtain the titanium nitride-alumina composite granule through Processing of Preparation such as pulverizing, grind, 100 orders sieve with heat-up rate.With the powder body material that obtains at the dry-pressing formed processing of the condition of 20MPa 15s; The back is carried out isostatic cool pressing processing 90s and is obtained ceramic body under 200MPa; Be placed in the nitrogen atmosphere stove; With heat-up rate is that 5 ℃/min is warming up to 1500 ℃ of insulations 5 hours, takes out behind the naturally cooling and promptly obtains titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material.
By the titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material that the foregoing description 8 prepares, its thing that mainly exists is titanium nitride, aluminum oxide and a spot of MgAl mutually
2O
4And bytownite, its strength at normal temperature value is 593.1MPa, the fracture toughness property value is 5.27MPam
1/2
Claims (6)
1. the preparation method of a titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material; It is characterized in that: in total batching quality
aluminium ash; And
rutile breeze or Rutile type Titanium Dioxide are raw material; Prepare the sample base substrate through batching, ball milling, technological process such as dry-pressing formed; Base substrate after the moulding is warming up to 1100 ℃～1500 ℃, is incubated 0.1 hour～100 hours in Reaktionsofen under nitrogen atmosphere, prepare the titanium nitride-alumina composite powder material; Then the powder body material that obtains is obtained the complex phase ceramic base substrate through processing such as dry-pressing formed, isostatic cool pressings; The gained base substrate is warming up to 1400 ℃～1800 ℃, is incubated 0.1 hour～100 hours under nitrogen atmosphere, obtain titanium nitride-alumina multi-phase wear-resistant refractory ceramics behind the naturally cooling in Reaktionsofen.
2. preparation method according to claim 1 is characterized in that: the main chemical compositions of aluminium ash is that Al content is 5～30wt.%, Al
2O
3Content is that 5～20wt.%, AlN content are 10～30wt.%, MgAl
2O
4Content is 10～40wt.%, SiO
2Content is that 1～10wt.%, NaCl content are that 1～10wt.%, CaO content are 1～10wt.%, TiO
2Content is 1～10wt%, Fe
2O
3Content is 1～10wt.%, and its particle diameter is less than 200 μ m.
3. preparation method according to claim 1 is characterized in that: the staple of rutile breeze or Rutile type Titanium Dioxide is TiO
2, its content is 85wt.%～99wt.%, particle diameter is less than 100 μ m.
4. preparation method according to claim 1 is characterized in that: the pressure of dry-pressing formed processing is 0.1～60MPa, and the pressure action time is 10～60s; The pressure that isostatic cool pressing is handled is 150～300MPa, and the pressure action time is 60～120s.
5. preparation method according to claim 1 is characterized in that: Reaktionsofen or for atmosphere furnace or for electric arc furnace or for induction furnace.
6. preparation method according to claim 1 is characterized in that: described nitrogen atmosphere pressure is
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210318895.4A CN102826852B (en) | 2012-08-31 | 2012-08-31 | A kind of preparation method of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210318895.4A CN102826852B (en) | 2012-08-31 | 2012-08-31 | A kind of preparation method of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102826852A true CN102826852A (en) | 2012-12-19 |
| CN102826852B CN102826852B (en) | 2016-01-13 |
Family
ID=47330195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210318895.4A Expired - Fee Related CN102826852B (en) | 2012-08-31 | 2012-08-31 | A kind of preparation method of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102826852B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112374472A (en) * | 2020-10-17 | 2021-02-19 | 北京科技大学 | Titanium nitride coated Ti2O3Composite Al2O3Material and method for the production thereof |
| CN113307292A (en) * | 2021-07-02 | 2021-08-27 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-strength, superhard and wear-resistant brown corundum containing titanium nitride |
| CN117842942A (en) * | 2024-01-10 | 2024-04-09 | 浙江能鹏半导体材料有限责任公司 | A method for preparing nano aluminum nitride powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349950A (en) * | 2001-11-30 | 2002-05-22 | 中国科学院上海硅酸盐研究所 | Prepn of conductive composite nanometer titanium nitride-alumina material |
| CN1958515A (en) * | 2006-10-30 | 2007-05-09 | 陕西科技大学 | Method for preparing TiN/Al2O3 composite materials |
| CN101654371A (en) * | 2009-09-18 | 2010-02-24 | 中国地质大学（北京） | Magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material and preparation method thereof |
| CN101654373A (en) * | 2009-09-18 | 2010-02-24 | 中国地质大学（北京） | Method for preparing Fe-Sialon spinel complex phase fire-proof material |
| CN101857425A (en) * | 2010-06-23 | 2010-10-13 | 哈尔滨工业大学 | Al2O3-TiN matrix composite material for time-of-flight detector and its preparation method |
-
2012
- 2012-08-31 CN CN201210318895.4A patent/CN102826852B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349950A (en) * | 2001-11-30 | 2002-05-22 | 中国科学院上海硅酸盐研究所 | Prepn of conductive composite nanometer titanium nitride-alumina material |
| CN1958515A (en) * | 2006-10-30 | 2007-05-09 | 陕西科技大学 | Method for preparing TiN/Al2O3 composite materials |
| CN101654371A (en) * | 2009-09-18 | 2010-02-24 | 中国地质大学（北京） | Magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material and preparation method thereof |
| CN101654373A (en) * | 2009-09-18 | 2010-02-24 | 中国地质大学（北京） | Method for preparing Fe-Sialon spinel complex phase fire-proof material |
| CN101857425A (en) * | 2010-06-23 | 2010-10-13 | 哈尔滨工业大学 | Al2O3-TiN matrix composite material for time-of-flight detector and its preparation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112374472A (en) * | 2020-10-17 | 2021-02-19 | 北京科技大学 | Titanium nitride coated Ti2O3Composite Al2O3Material and method for the production thereof |
| CN112374472B (en) * | 2020-10-17 | 2022-04-29 | 北京科技大学 | Titanium nitride coated Ti2O3Composite Al2O3Material and method for the production thereof |
| CN113307292A (en) * | 2021-07-02 | 2021-08-27 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-strength, superhard and wear-resistant brown corundum containing titanium nitride |
| CN117842942A (en) * | 2024-01-10 | 2024-04-09 | 浙江能鹏半导体材料有限责任公司 | A method for preparing nano aluminum nitride powder |
| CN117842942B (en) * | 2024-01-10 | 2025-11-11 | 浙江能鹏半导体材料有限责任公司 | Preparation method of nano aluminum nitride powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102826852B (en) | 2016-01-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101914639A (en) | A method for on-line recovery of iron from iron-containing industrial slag and preparation of glass-ceramic frit | |
| CN102557683A (en) | Aluminum chrome refractory material | |
| CN104788112B (en) | A kind of electro-corundum material and production method thereof | |
| CN101823889B (en) | Anhydrous stemming and preparation method thereof | |
| CN101775492B (en) | Method for producing silicon-aluminum-ferroalloy by utilizing aluminum ash and copper slag | |
| CN106145686B (en) | A kind of complicated utilization Pb-Zn tailings, devitrified glass of electrolytic manganese waste residue and preparation method thereof | |
| CN107555435A (en) | A kind of method that carbon thermal reduction titanium-containing blast furnace slag prepares titanium carbide | |
| CN101503302A (en) | Carboneous fire-resistant material for furnace brick lining and preparation thereof | |
| CN104402462B (en) | A kind of stopper and technique thereof producing mineral wool flow control for blast furnace slag | |
| CN102584181B (en) | Method for preparing periclase-silicon carbide-carbon composite powder through in-situ reaction | |
| CN102826852A (en) | Preparation method of titanium nitride-alumina complex phase wear resistant high-temperature resistant ceramics material | |
| CN102851427A (en) | Method for online production of sponge iron by using steel residue waste heat | |
| CN103449826B (en) | Preparation method of gunning mix for kiln repair | |
| CN101988614B (en) | Preparation method of ceramic-lined composite steel pipe | |
| CN110156445A (en) | A kind of rotary hearth furnace high-strength wear-resistant pouring material and preparation method thereof | |
| CN104387093B (en) | A kind of mouth of a river and production technology thereof producing mineral wool flow control for blast furnace slag | |
| CN101234902A (en) | Method for Synthesizing α-Sialon Ceramic Material Using Aluminum Ash and Blast Furnace Slag | |
| CN102424586A (en) | A kind of preparation method of SiC refractory raw material powder | |
| CN104844216B (en) | A kind of Sialon-MgAl2o4-SiC multi-phase wear-resistant ceramic material and preparation method thereof | |
| CN100408510C (en) | Process of preparing heterogenous conducting Si3N4/Tin ceramic material tail iron ore | |
| CN105503193B (en) | It is a kind of to prepare Sialon/Si using kyanite milltailings transition phase inversion3N4The preparation method of-SiC complex phase high-temperature resistant materials | |
| CN101654373A (en) | Method for preparing Fe-Sialon spinel complex phase fire-proof material | |
| CN104557094A (en) | Method for preparing mullite aggregate for high-alumina refractory bricks by taking high-aluminum pulverized fuel ash as single aluminum source | |
| CN102584189A (en) | Method for manufacturing alkali complex-phase high-temperature resistant powder containing forsterite-silicon nitride-silicon carbide | |
| CN109020516A (en) | A kind of baking of Novel free can repair chute |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160113 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |