CN102584245B - Preparation method of aluminium nitride and titanium diboride composite ceramic - Google Patents
Preparation method of aluminium nitride and titanium diboride composite ceramic Download PDFInfo
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- CN102584245B CN102584245B CN 201210039325 CN201210039325A CN102584245B CN 102584245 B CN102584245 B CN 102584245B CN 201210039325 CN201210039325 CN 201210039325 CN 201210039325 A CN201210039325 A CN 201210039325A CN 102584245 B CN102584245 B CN 102584245B
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Abstract
The invention relates to the field of ceramic preparation technology, and in particular relates to a preparation method of aluminium nitride and titanium diboride composite ceramic. The preparation method comprises the steps of: firstly, mixing 60-95wt% of boron nitride and 5-40wt% of titanium diboride to prepare an ingredient; adding a bonding agent into the ingredient, and preparing blank by evenly mixing; then, sieving the blank and molding by pressing; then heating the blank which is molded by pressing to 1600-1900 DEG C from room temperature under the vacuum condition, and sintering for 1-4h; finally, cooling the blank along a furnace to prepare a prefabricate of boron nitride and titanium diboride; putting the prefabricate into a crucible, and arranging an Al ingot at the upper part of the prefabricate, wherein the mass of the Al ingot is 160-200% of that of the prefabricate; heating to 1100-1300 DEG C from the room temperature under the vacuum condition; carrying out heat preservation for 2-8h; leading Al to infiltrate into the prefabricate of boron nitride and titanium diboride; and cooling to the room temperature along the furnace to prepare the aluminium nitride and titanium diboride composite ceramic.
Description
Technical field
The present invention relates to the ceramics processing field, be specifically related to the preparation method of a kind of aluminium nitride and TiB2 composite ceramics.
Background technology
Do not see as yet both at home and abroad at present and utilize the vacuum metal method of impregnation to prepare aluminium nitride and TiB2 (AlN/TiB
2) any report of composite ceramics.Aluminium nitride and TiB2 (AlN/TiB
2) preparation technology of composite ceramics mainly contains: (1) is with AlN, TiB
2Hot pressed sintering for raw material; (2) be the reaction hot-pressing sintering of raw material with Al, TiH and BN or with Al, TiN and BN; (3) with AlN, TiB
2And Y
2O
3Spark plasma sintering for raw material; (4) with AlN, TiB
2And Y
2O
3Microwave sintering for raw material; (5) AlN, TiB
2And Y
2O
3Gas pressure sintering for raw material; The AlN/TiB that above method can be prepared
2Composite ceramic material, but raw materials cost height, complex process also has (6) in addition with Al, N
2And TiB
2For gas phase HIP sintering etc. is synthesized in the burning of raw material; Though this method reaction times is short, the fast sintered products poor reproducibility of preparation speed is not suitable for industrial-scale production.And present method is for aluminium nitride and TiB2 (AlN/TiB
2) preparation technology of composite ceramics is simple, cost of material is cheap, and the prospect of can operating is extensive.
Summary of the invention
The objective of the invention is the deficiency at the prior art existence, the preparation method of a kind of aluminium nitride and TiB2 composite ceramics is provided.
Technical scheme of the present invention is undertaken by following two processing steps:
The first step, prepare boron nitride and titanium diboride precast body: at first the boron nitride of 60 ~ 95wt% is mixed with the titanium diboride of 5 ~ 40wt%, make batching, add bonding agent and mix and make blank in batching again, after being sieved, blank is pressed, then with compressing blank after being warmed up to 1600 ~ 1900 ℃ with the programming rate of 10 ~ 40 ℃/min from room temperature under vacuum condition, sintering 1 ~ 4 hour, make finally the blank after sintering cool to room temperature with the furnace, prepare boron nitride and titanium diboride precast body
Second step, the preparation of aluminium nitride and TiB2 composite ceramics: boron nitride and the TiB2 precast body of the first step preparation are put into crucible, and be that 160 ~ 200% Al ingot of precast body quality is placed on boron nitride and TiB2 precast body top with quality, under vacuum condition, after being warmed up to 1100 ~ 1300 ℃ with the heat-up rate of 10 ~ 40 ℃/min from room temperature, be incubated 2 ~ 8 hours, after making Al be infiltrated up in boron nitride and the TiB2 precast body, cool to room temperature with the furnace, prepare aluminium nitride and TiB2 composite ceramics;
Described boron nitride adopts with mixing of TiB2 and does the mode of mixing, and mixes 8 ~ 24 hours;
Described caking agent is resol-acetone saturated solution at room temperature, and its add-on is 2 ~ 15% of the batching quality;
The order number that described blank sieves is 60 ~ 100 orders;
Described blank compression moulding pressure is 100 ~ 200 MPa, pressurize 1min;
It is to carry out under vacuum tightness is lower than the condition of 50Pa that described blank with compression moulding carries out sintering;
It is to carry out under vacuum tightness is lower than the condition of 50Pa that the described Al of making is infiltrated up in boron nitride and the TiB2 precast body.
Compare with technology with existing, characteristics of the present invention and beneficial effect thereof are:
1. take full advantage of the BN that output is big, cost is cheap relatively and Al ingot as main raw material, therefore, controlled production cost effectively;
2. the present invention is owing to utilize the vacuum metal Infiltration Technics, make and both reduced the interference of oxygen to producing, Al is fully contacted with BN, the interface contact range is wide, and infiltration temperature not only can be offered help for the flowability of metal A l and satisfied Al and BN reaction just and generate AlN thermodynamics basis, make Al and BN surface reaction fully and effective.Simultaneously because the TiB that adds
2Increase, make a small amount of AlB that surface reaction produces thereupon
12Particle size obviously reduces, and has reduced effectively between the particle because the bifurcated cracking phenomena that the external load adding causes easily makes mechanical property obviously increase;
3. be prepared into the power height, the repetition rate height, product impurity is few;
4. this product has premium properties: (1) high compactness: the density of composite ceramics product is all more than 99%; (2) mechanical property excellence: folding strength is 51.77 ~ 284.03MPa, and fracture toughness property is 2.91 ~ 4.63 MPa ﹒ m
1/2, hardness (HRC) is 50 ~ 73.5; (3) owing to contain conductive material TiB
2, make that workabilitys such as line cutting are strong.
Description of drawings
Fig. 1, the aluminium nitride of embodiment 3 preparation and the microstructure photograph of TiB2 composite ceramics, 1 AlN wherein, 2 TiB
2, 3 AlB
12
Embodiment
Elaborate below in conjunction with the present invention of embodiment, but protection scope of the present invention is not limited only to following embodiment:
The unit type that following embodiment adopts is: vacuum carbon tube furnace is the ZRS-200 type; The omnipotent sample machine of WE-10A fluid pressure type; X
,Pert Pro MRD diffractometer; The Leica metaloscope; S-3400N type scanning electronic microscope.
Embodiment 1:
The first step, preparation boron nitride and TiB2 precast body: at first the boron nitride of 95g is mixed with the TiB2 of 5g, make batching, and put into the spheroidal graphite jar and mixed 24 hours, add resol-acetone saturated solution under the room temperature account for batching quality 5% again in the batching as caking agent, and mix, make blank, make blank cross 60 mesh sieves then, will sieve good blank then and put into punching block, place an order in 100MPa and axially suppress 1min, form the round base of Ф 30mm, the base cake that mold pressing is good is packed in the plumbago crucible, places vacuum carbon tube furnace, under the condition of vacuum tightness 47Pa, after being warmed up to 1600 ℃ with the heat-up rate of 10 ℃/min from room temperature, sintering 1 hour makes the blank behind the sintering cool to room temperature with the furnace at last
Second step, the preparation of aluminium nitride and TiB2 composite ceramics: boron nitride and the TiB2 precast body of the first step preparation are put into crucible, and be that 160% Al ingot of precast body quality is placed on precast body top with quality, under the condition of vacuum tightness 47Pa, after being warmed up to 1100 ℃ with the heat-up rate of 10 ℃/min from room temperature, be incubated 2 hours, make Al be infiltrated up in boron nitride and the TiB2 precast body after, cool to room temperature with the furnace, prepare aluminium nitride and TiB2 composite ceramics;
Detected result shows: the aluminium nitride of preparation and TiB2 (AlN/TiB
2) the main thing of composite ceramics is AlN, TiB mutually
2, a spot of AlB
12Micro-BN with remnants.The density 99.3% of this composite ceramic material, folding strength are 51.77MPa, and fracture toughness property is 2.91MPam
1/2, Rockwell hardness (HRC) is 58.5.
Embodiment 2:
The first step, preparation boron nitride and TiB2 precast body: at first the boron nitride of 60g is mixed with the TiB2 of 40g, make batching, and put into the spheroidal graphite jar and mixed 16 hours, add resol-acetone saturated solution under the room temperature account for batching quality 10% again in the batching as caking agent, and mix, make blank, make blank cross 100 mesh sieves then, will sieve good blank then and put into punching block, place an order in 180MPa and axially suppress 1min, form the round base of Ф 30mm, the base cake that mold pressing is good is packed in the plumbago crucible, places vacuum carbon tube furnace, under the condition of vacuum tightness 48Pa, after being warmed up to 1700 ℃ with the heat-up rate of 20 ℃/min from room temperature, sintering 2 hours makes the blank behind the sintering cool to room temperature with the furnace at last
Second step, the preparation of aluminium nitride and TiB2 composite ceramics: boron nitride and the TiB2 precast body of the first step preparation are put into crucible, and be that the Al ingot of precast body quality 200% is placed on precast body top with quality, under the condition of vacuum tightness 48Pa, after being warmed up to 1100 ℃ with the heat-up rate of 20 ℃/min from room temperature, be incubated 8 hours, make Al be infiltrated up in boron nitride and the TiB2 precast body after, cool to room temperature with the furnace, prepare aluminium nitride and TiB2 composite ceramics;
Detected result shows: the aluminium nitride of preparation and TiB2 (AlN/TiB
2) the main thing of composite ceramics is AlN, TiB mutually
2, a spot of AlB
12Trace of Al with remnants.The density 99.1% of this composite ceramic material, folding strength are 284.03MPa, and fracture toughness property is 4.63MPam
1/2, Rockwell hardness (HRC) is 73.5.
Embodiment 3:
The first step, preparation boron nitride and TiB2 precast body: at first the boron nitride of 80g is mixed with the TiB2 of 20g, make batching, and put into the spheroidal graphite jar and mixed 12 hours, add resol-acetone saturated solution under the room temperature account for batching quality 15% again in the batching as caking agent, and mix, make blank, make blank cross 80 mesh sieves then, will sieve good blank then and put into punching block, place an order in 150MPa and axially suppress 1min, form the round base of Ф 30mm, the base cake that mold pressing is good is packed in the plumbago crucible, places vacuum carbon tube furnace, under the condition of vacuum tightness 49Pa, after being warmed up to 1800 ℃ with the heat-up rate of 30 ℃/min from room temperature, sintering 3 hours makes the blank behind the sintering cool to room temperature with the furnace at last
Second step, the preparation of aluminium nitride and TiB2 composite ceramics: boron nitride and the TiB2 precast body of the first step preparation are put into crucible, and be that 180% Al ingot of precast body quality is placed on precast body top with quality, under the condition of vacuum tightness 49Pa, after being warmed up to 1300 ℃ with the heat-up rate of 30 ℃/min from room temperature, be incubated 4 hours, make Al be infiltrated up in boron nitride and the TiB2 precast body after, cool to room temperature with the furnace, prepare aluminium nitride and TiB2 composite ceramics;
Detected result shows: the aluminium nitride of preparation and TiB2 (AlN/TiB
2) the main thing of composite ceramics is AlN, TiB mutually
2, a spot of AlB
12The density 99.2% of this composite ceramic material, folding strength are 125.58MPa, and fracture toughness property is 3.85MPam
1/2, Rockwell hardness (HRC) is 50.
Embodiment 4:
The first step, preparation boron nitride and TiB2 precast body: at first the boron nitride of 70g is mixed with the TiB2 of 30g, make batching, and put into the spheroidal graphite jar and mixed 8 hours, add resol-acetone saturated solution under the room temperature account for batching quality 2% again in the batching as caking agent, and mix, make blank, make blank cross 60 mesh sieves then, will sieve good blank then and put into punching block, place an order in 200MPa and axially suppress 1min, form the round base of Ф 30mm, the base cake that mold pressing is good is packed in the plumbago crucible, places vacuum carbon tube furnace, under the condition of vacuum tightness 45Pa, after being warmed up to 1900 ℃ with the heat-up rate of 40 ℃/min from room temperature, sintering 4 hours makes the blank behind the sintering cool to room temperature with the furnace at last
Second step, the preparation of aluminium nitride and TiB2 composite ceramics: boron nitride and the TiB2 precast body of the first step preparation are put into crucible, and be that 170% Al ingot of precast body quality is placed on precast body top with quality, under the condition of vacuum tightness 45Pa, after being warmed up to 1300 ℃ with the heat-up rate of 40 ℃/min from room temperature, be incubated 6 hours, make Al be infiltrated up in boron nitride and the TiB2 precast body after, cool to room temperature with the furnace, prepare aluminium nitride and TiB2 composite ceramics;
Detected result shows: the aluminium nitride of preparation and TiB2 (AlN/TiB
2) the main thing of composite ceramics is AlN, TiB mutually
2, a spot of AlB
12The density of this composite ceramic material is 99.1%, and folding strength is 209MPa, and fracture toughness property is 4.33MPam
1/2, Rockwell hardness (HRC) is 57.
Claims (5)
1. the preparation method of an aluminium nitride and TiB2 composite ceramics is characterized in that being undertaken by following two steps:
The first step, prepare boron nitride and titanium diboride precast body: at first the boron nitride of 60 ~ 95wt% is mixed with the titanium diboride of 5 ~ 40wt%, make batching, add bonding agent and mix and make blank in batching again, after being sieved, blank is pressed, then with compressing blank at low vacuum after being warmed up to 1600 ~ 1900 ℃ with the programming rate of 10 ~ 40 ℃/min from room temperature under the condition of 50Pa, sintering 1 ~ 4 hour, make finally the blank after sintering cool to room temperature with the furnace, prepare boron nitride and titanium diboride precast body
Second step, the preparation of aluminium nitride and TiB2 composite ceramics: boron nitride and the TiB2 precast body of the first step preparation are put into crucible, and be that 160 ~ 200% Al ingot of precast body quality is placed on boron nitride and TiB2 precast body top with quality, be lower than in vacuum tightness under the condition of 50Pa, after being warmed up to 1100 ~ 1300 ℃ with the heat-up rate of 10 ~ 40 ℃/min from room temperature, be incubated 2 ~ 8 hours, after making Al be infiltrated up in boron nitride and the TiB2 precast body, cool to room temperature with the furnace, prepare aluminium nitride and TiB2 composite ceramics.
2. the preparation method of a kind of aluminium nitride according to claim 1 and TiB2 composite ceramics is characterized in that adopting the dried mode of mixing mixing of described boron nitride and TiB2, mixes 8 ~ 24 hours.
3. the preparation method of a kind of aluminium nitride according to claim 1 and TiB2 composite ceramics is characterized in that described caking agent is resol-acetone saturated solution at room temperature, and its add-on is 2 ~ 15% of the batching quality.
4. the preparation method of a kind of aluminium nitride according to claim 1 and TiB2 composite ceramics is characterized in that the order number that described blank sieves is 60 ~ 100 orders.
5. the preparation method of a kind of aluminium nitride according to claim 1 and TiB2 composite ceramics is characterized in that described blank compression moulding pressure is 100 ~ 200 MPa, pressurize 1min.
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| CN101708989A (en) * | 2009-12-14 | 2010-05-19 | 哈尔滨工业大学 | Method for preparing aluminum nitride/boron nitride composite ceramic through combustion synthesis method |
| CN101723678A (en) * | 2009-12-14 | 2010-06-09 | 哈尔滨工业大学 | Method for preparing novel conductive ceramic evaporation boat by combustion synthesis |
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| CN101708989A (en) * | 2009-12-14 | 2010-05-19 | 哈尔滨工业大学 | Method for preparing aluminum nitride/boron nitride composite ceramic through combustion synthesis method |
| CN101723678A (en) * | 2009-12-14 | 2010-06-09 | 哈尔滨工业大学 | Method for preparing novel conductive ceramic evaporation boat by combustion synthesis |
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