CN103420676A - High compactness and high thermal shock resistance composite material and preparation method thereof - Google Patents

High compactness and high thermal shock resistance composite material and preparation method thereof Download PDF

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Publication number
CN103420676A
CN103420676A CN2013103241359A CN201310324135A CN103420676A CN 103420676 A CN103420676 A CN 103420676A CN 2013103241359 A CN2013103241359 A CN 2013103241359A CN 201310324135 A CN201310324135 A CN 201310324135A CN 103420676 A CN103420676 A CN 103420676A
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powder
matrix material
fine
heat resistance
shock resistant
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严密
徐崟
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a high compactness and high thermal shock resistance composite material and a preparation method thereof. The composite material comprises the following components by weight percent: 50-85 percent of BN, 5-30 percent of ZrO2, 3-30 percent of Al2O3, 2-30 percent of Si3N4 and 5 percent of sintering aids, wherein BN is taken as the substrate, and ZrO2, Al2O3 and Si3N4 are taken as additives. The preparation method of the composite material comprises the following steps: placing mixed powder in a ball grinding tank according to the formula, performing ball grinding for 1-20 hours, drying, sifting, then prilling through static pressure, placing the mixture in a graphite die, heating the mixture in a hot press furnace with N2 to reach 1700-1900 DEG C, and keeping warm for 10-90 minutes; the hot-press pressure is 10-50MPa. The composite material prepared by the method is high in strength, very excellent in thermal shock resistance and oxidation resistance, uniform in structure, and high in overall reliability; the method disclosed by the invention has the advantages that the sintering temperature is low, the sintering time is short, the process is simple, and the cost is low.

Description

A kind of high fine and close high-heat resistance shock resistant matrix material and preparation method thereof
Technical field
The present invention relates to the high-temperature structural material field, be specifically related to a kind of high fine and close high-heat resistance shock resistant matrix material and preparation method thereof.
Background technology
The related industries such as modern metallurgy need high-temperature structural material to have excellent over-all properties, wherein especially important with mechanical property, heat-shock resistance, oxidation-resistance and machinable.Hexagonal boron nitride, as a kind of high-temperature structural material, has good high thermal resistance, erosion resistance, stability at elevated temperature and heat-shock resistance, especially has outstanding machinable, therefore is widely used in the related industrieies such as metallurgical.But its mechanical property and oxidation-resistance are poor, and, B atom in h-BN and O atom are by strong covalent bonds, very low of its self-diffusion coefficient, sheet BN easily forms card form bridging structure when high temperature sintering, therefore h-BN is difficult to densified sintering product, and this has also reduced its mechanical property and oxidation-resistance to a certain extent, has further limited its application.
Current patent both domestic and external is mainly to assign to improve the mechanical property of BN material by adding high-intensity one-tenth, but has but reduced to a certain extent the heat-shock resistance of BN material, is unfavorable for the application under its high temperature.And the research of the domestic and international oxidation-resistance about raising BN material and technology of preparing aspect is very rare.Therefore, obtain a kind of mechanical property, heat-shock resistance and oxidation-resistance all very excellent BN material seem particularly urgent.
For obtaining all very excellent BN materials of a kind of mechanical property, heat-shock resistance, the present invention selects several additives, when improving the BN strength of materials, further improved its heat-shock resistance, utilize simple production technique, prepare the fine and close high-heat resistance shock resistant matrix material of height that over-all properties is very excellent, fill up the domestic and international blank in this one side.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of high fine and close high-heat resistance shock resistant matrix material and preparation method thereof is provided.
Technical scheme of the present invention is:
High fine and close high-heat resistance shock resistant matrix material be take BN as matrix, ZrO 2, Al 2O 3, Si 3N 4For additive, by weight percentage, wherein BN is 50-85%, ZrO 2For 5-30%, Al 2O 3For 3-30%, Si 3N 4For 2-30%, sintering agent is 5%.
The preferred content of described BN is 60-85%.
ZrO 2Preferred content be 10-30%.
Al 2O 3Preferred content be 5-20%.
Si 3N 4Preferred content be 2-20%.
The preparation method's of high fine and close high-heat resistance shock resistant matrix material step is as follows:
1) weight percent is respectively to the BN of 50-85%, the ZrO of 5-30% 2, the Al of 3-30% 2O 3, the Si of 2-30% 3N 4And 5% sintering agent powder is mixed to get initial powder;
2) initial powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 1-20 hour is dried in baking oven;
3) powder of oven dry is sieved, under 2-80MPa, the static pressure granulation obtains base substrate;
4) base substrate fragmentation static pressure obtained, cross the 30-50 mesh sieve and obtain powder;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1700-1900 ℃ with the temperature rise rate of 10-30 ℃/min, insulation 10-90min, hot pressing pressure is 10-50MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
During ball milling, ratio of grinding media to material is 3-15:1.
BN powder mean particle sizes after step 3) is sieved is 0.5-5 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 1-10 μ m.
The beneficial effect that the present invention compared with prior art has:
1) the fine and close high-heat resistance shock resistant composite material strength of the height for preparing is high, and heat-shock resistance and antioxidant property all very excellent, even structure, global reliability is high;
2) sintering temperature is low, and sintering time is short, and technique is simple, and cost is low.
Embodiment
Embodiment 1
1) weight percent is respectively to 85% BN, 5% ZrO 2, 3% Al 2O 3, 2% Si 3N 4Powder and 5% sintering agent powder evenly mix;
2) mixed powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 1 hour is dried in baking oven, and gained BN powder mean particle sizes is 5 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 10 μ m;
3) powder of oven dry is sieved, static pressure granulation under 2MPa;
4) base substrate fragmentation static pressure obtained, cross 30 mesh sieves;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1700 ℃ with the temperature rise rate of 10 ℃/min, insulation 10min, hot pressing pressure is 10MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
Test batching purity used and be technical pure, the fine and close high-heat resistance shock resistant matrix material of the height that obtains relative density is 90%, and ultimate compression strength is 175MPa, and folding strength is 74MPa, Critical thermal shock temperature difference Δ Tc > 1000 ℃.
Embodiment 2
1) weight percent is respectively to 65% BN, 15% ZrO 2, 3% Al 2O 3, 2% Si 3N 4Powder and 5% sintering agent powder evenly mix;
2) mixed powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 5 hours is dried in baking oven, and gained BN powder mean particle sizes is 3 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 5 μ m;
3) powder of oven dry is sieved, static pressure granulation under 20MPa;
4) base substrate fragmentation static pressure obtained, cross 50 mesh sieves;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1700 ℃ with the temperature rise rate of 20 ℃/min, insulation 30min, hot pressing pressure is 20MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
Test batching purity used and be technical pure, the fine and close high-heat resistance shock resistant matrix material of the height that obtains relative density is 94%, and ultimate compression strength is 245MPa, and folding strength is 97MPa, Critical thermal shock temperature difference Δ Tc > 1200 ℃.
Embodiment 3
1) weight percent is respectively to 60% BN, 30% ZrO 2, 3% Al 2O 3, 2% Si 3N 4Powder and 5% sintering agent powder evenly mix;
2) mixed powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 10 hours is dried in baking oven, and gained BN powder mean particle sizes is 1 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 3 μ m;
3) powder of oven dry is sieved, static pressure granulation under 40MPa;
4) base substrate fragmentation static pressure obtained, cross 40 mesh sieves;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1800 ℃ with the temperature rise rate of 20 ℃/min, insulation 30min, hot pressing pressure is 30MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
Test batching purity used and be technical pure, the fine and close high-heat resistance shock resistant matrix material of the height that obtains relative density is 95%, and ultimate compression strength is 316MPa, and folding strength is 126MPa, Critical thermal shock temperature difference Δ Tc > 1300 ℃.
Embodiment 4
1) weight percent is respectively to 70% BN, 10% ZrO 2, 10% Al 2O 3, 5% Si 3N 4Powder and 5% sintering agent powder evenly mix;
2) mixed powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 15 hours is dried in baking oven, and gained BN powder mean particle sizes is 1 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 2 μ m;
3) powder of oven dry is sieved, static pressure granulation under 60MPa;
4) base substrate fragmentation static pressure obtained, cross 30 mesh sieves;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1800 ℃ with the temperature rise rate of 20 ℃/min, insulation 60min, hot pressing pressure is 30MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
Test batching purity used and be technical pure, the fine and close high-heat resistance shock resistant matrix material of the height that obtains relative density is 94%, and ultimate compression strength is 219MPa, and folding strength is 92MPa, Critical thermal shock temperature difference Δ Tc > 1200 ℃.
Embodiment 5
1) weight percent is respectively to 60% BN, 5% ZrO 2, 30% Al 2O 3, 2% Si 3N 4Powder and 5% sintering agent powder evenly mix;
2) mixed powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 15 hours is dried in baking oven, and gained BN powder mean particle sizes is 1 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 2 μ m;
3) powder of oven dry is sieved, static pressure granulation under 60MPa;
4) base substrate fragmentation static pressure obtained, cross 50 mesh sieves;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1850 ℃ with the temperature rise rate of 20 ℃/min, insulation 60min, hot pressing pressure is 40MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
Test batching purity used and be technical pure, the fine and close high-heat resistance shock resistant matrix material of the height that obtains relative density is 96%, and ultimate compression strength is 198MPa, and folding strength is 85MPa, Critical thermal shock temperature difference Δ Tc > 1100 ℃.
Embodiment 6
1) weight percent is respectively to 50% BN, 5% ZrO 2, 10% Al 2O 3, 30% Si 3N 4Powder and 5% sintering agent powder evenly mix;
2) mixed powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 20 hours is dried in baking oven, and gained BN powder mean particle sizes is 0.5 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 1 μ m;
3) powder of oven dry is sieved, static pressure granulation under 80MPa;
4) base substrate fragmentation static pressure obtained, cross 30 mesh sieves;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1900 ℃ with the temperature rise rate of 30 ℃/min, insulation 90min, hot pressing pressure is 50MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
Test batching purity used and be technical pure, the fine and close high-heat resistance shock resistant matrix material of the height that obtains relative density is 97%, and ultimate compression strength is 310MPa, and folding strength is 98MPa, Critical thermal shock temperature difference Δ Tc > 1100 ℃.

Claims (8)

1. one kind high fine and close high-heat resistance shock resistant matrix material, it is characterized in that: this matrix material be take BN as matrix, ZrO 2, Al 2O 3, Si 3N 4For additive, by weight percentage, wherein BN is 50-85%, ZrO 2For 5-30%, Al 2O 3For 3-30%, Si 3N 4For 2-30%, sintering agent is 5%.
2. according to the fine and close high-heat resistance shock resistant matrix material of height claimed in claim 1, it is characterized in that: the content of described BN is 60-85%.
3. according to the fine and close high-heat resistance shock resistant matrix material of height claimed in claim 1, it is characterized in that: described ZrO 2Content be 10-30%.
4. according to the fine and close high-heat resistance shock resistant matrix material of height claimed in claim 1, it is characterized in that: described Al 2O 3Content be 5-20%.
5. according to the fine and close high-heat resistance shock resistant matrix material of height claimed in claim 1, it is characterized in that: described Si 3N 4Content be 2-20%.
6. the preparation method of a high fine and close high-heat resistance shock resistant matrix material, is characterized in that, comprises the steps:
1) weight percent is respectively to the BN of 50-85%, the ZrO of 5-30% 2, the Al of 3-30% 2O 3, the Si of 2-30% 3N 4And 5% sintering agent powder is mixed to get initial powder;
2) initial powder is placed in to ball grinder, usings ethanol as dispersion agent, ball milling 1-20 hour is dried in baking oven;
3) powder of oven dry is sieved, under 2-80MPa, the static pressure granulation obtains base substrate;
4) base substrate fragmentation static pressure obtained, cross the 30-50 mesh sieve and obtain powder;
5) powder directly is positioned in graphite jig, is being connected with N 2Hot pressing furnace in rise to 1700-1900 ℃ with the temperature rise rate of 10-30 ℃/min, insulation 10-90min, hot pressing pressure is 10-50MPa, is fired into high fine and close high-heat resistance shock resistant matrix material.
7. according to the preparation method of the fine and close high-heat resistance shock resistant matrix material of height claimed in claim 6, it is characterized in that: during ball milling, ratio of grinding media to material is 3-15:1.
8. according to the preparation method of the fine and close high-heat resistance shock resistant matrix material of height claimed in claim 6, it is characterized in that: the BN powder mean particle sizes after step 3) is sieved is 0.5-5 μ m, ZrO 2, Al 2O 3, Si 3N 4Powder mean particle sizes is 1-10 μ m.
CN2013103241359A 2013-07-30 2013-07-30 High compactness and high thermal shock resistance composite material and preparation method thereof Pending CN103420676A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105753485A (en) * 2015-12-11 2016-07-13 天津城建大学 Boron nitride composite ceramic material and pressureless sintering process thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1518844A1 (en) * 2003-09-25 2005-03-30 Sumitomo Metal Industries, Ltd. Machinable ceramic
JP2009029681A (en) * 2007-07-30 2009-02-12 Mitsui Kozan Material Kk Method for producing free-cutting ceramic
CN102557647A (en) * 2011-12-13 2012-07-11 河南富耐克超硬材料股份有限公司 Polycrystalline cubic boron nitride compound material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1518844A1 (en) * 2003-09-25 2005-03-30 Sumitomo Metal Industries, Ltd. Machinable ceramic
JP2009029681A (en) * 2007-07-30 2009-02-12 Mitsui Kozan Material Kk Method for producing free-cutting ceramic
CN102557647A (en) * 2011-12-13 2012-07-11 河南富耐克超硬材料股份有限公司 Polycrystalline cubic boron nitride compound material

Non-Patent Citations (1)

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Title
周张健: "《无机非金属材料工艺学》", 31 January 2010, 中国轻工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105753485A (en) * 2015-12-11 2016-07-13 天津城建大学 Boron nitride composite ceramic material and pressureless sintering process thereof
CN105753485B (en) * 2015-12-11 2018-09-28 天津城建大学 Boron nitride diphase ceramic material and its non-pressure sintering technology

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Application publication date: 20131204