CN1250762A - Process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter method - Google Patents

Process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter method Download PDF

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Publication number
CN1250762A
CN1250762A CN 99119429 CN99119429A CN1250762A CN 1250762 A CN1250762 A CN 1250762A CN 99119429 CN99119429 CN 99119429 CN 99119429 A CN99119429 A CN 99119429A CN 1250762 A CN1250762 A CN 1250762A
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hours
ball mill
powder
boron nitride
preparing boron
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CN 99119429
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Chinese (zh)
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曾照强
胡晓清
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Tsinghua University
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Tsinghua University
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Priority to CN 99119429 priority Critical patent/CN1250762A/en
Publication of CN1250762A publication Critical patent/CN1250762A/en
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Abstract

This invention relates to a method for preparing boron netride compound conductive ceramic evaporation vessel by using non-pressure sintering process. Firstly, the powder masses of raw materials are blended, the compounded powder material is mixed in ball mill, drying and sieving, the sieved material is heat-insulated in argon atmosphere furnace to proceed chemical reaction, the reacted-finished material is further pulverized in ball mill, after baking dry and sieving, it is prepressed into form, and then it is formed under cold and iso static pressure and final sintering so that the invented product is obtained. The evaporation vessel prepared by this invention has uniform resistance, the product qualification rate reaches 90%, it can be continuously used for 15 hrs and intermittently used up to 500 times, reaching the performance parameters of same category products abroad.

Description

The method of process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter
Conductive ceramic evaporation boat is the important heater element that is applied in the technology of vacuum metal film plating.The preparation process of conductive ceramic evaporation boat commonly used is that needed raw material is carried out mechanically mixing, while the powder shape that mixes is gone in the graphite jig to pressurize, heated and carry out sintering, the conductivity ceramics block after burned is carried out cutting processing.The skewness of the stupalith inner conductive phase that this preparation technology obtains makes that the yield rate of evaporation boat is low, unstable properties.
The objective of the invention is to propose a kind of method of process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter, in advance BN, Ti, three kinds of powders of Al are mixed by certain ratio row, reaction synthesizes the high BN-TiB of sintering activity in advance under 1200 ℃ temperature 2-AlN ceramic composite powders, and then carry out pressureless sintering is to make yield rate height, stable performance, conductive ceramic evaporation boat that price is low.
The method of process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter of the present invention comprises following each step:
(1) be that the following column weight amount of the material powder per-cent of 1~5 μ mixes mutually with granularity:
Silicon nitride: 40~60wt%
Titanium hydride: 20~30wt%
Aluminium powder: 10~30wt%
(2) with the powder of being prepared with weight ratio be: material: alcohol: ball mill mixing is carried out in ball=1: 1.5~2: 2~3, mixing time 10~15 hours;
(3) material that will mix was dried 10~15 hours down at 40~60 ℃, crossed 50~80 mesh standard sieves;
(4) material that will sieve is incubated 4~8 hours in 1000 ℃~1400 ℃ argon gas atmosphere stoves, carries out chemical reaction;
(5) material that will react carries out ball mill pulverizing again, and its ratio of grinding media to material is:
Material: alcohol: ball=1: 1.5~2: 2~3, under 40~60 ℃, dried 10~15 hours, cross 50~80 mesh standard sieves;
(6) material that will sieve gives moldedly, and pressure is 10~20MPa, then cold isostatic compaction under 150~250Mpa;
(7) base substrate that moulding is finished places nitrogen atmosphere, is heated to 1800~2000 ℃, burns 2~5 hours, is ceramic evaporation boat of the present invention.
The BN conductive ceramic evaporation boat of the present invention preparation has uniform resistance, and product qualified rate reaches 90%, resistivity range of variation can be from 300~2000 (micro-ohm. centimetre) regulate as required.The evaporation boat of preparation uses continuously and reaches 15 hours, is interrupted to use to reach 600 times, reaches external similar end properties parameter.Owing to adopted the pressureless sintering technology, improved single furnace output, product percent of pass also is improved, and has saved the machining process behind the sintering, and the price of evaporation boat is reduced greatly, is 20% of external like product, 50% of domestic like product.
Introduce embodiments of the invention below
Embodiment one
(1) takes by weighing BN 50%wt, TiH 220%wt, Al 30%wt, granularity is respectively 1 μ, 2 μ, 2 μ.
(2) in proportion with the powder prepared; Material: alcohol: ball=1: 1.5: 2 (weight), carried out ball mill mixing 12 hours.
(3) material that will mix is crossed 60 mesh sieves 50 ℃ of oven dry 12 hours.
(4) material that will sieve is incubated 5 hours in 1300 ℃ of argon atmospher stoves, carries out chemical reaction.
(5) material that will react carries out ball mill pulverizing again, and oven dry is sieved.
(6) powder that sieves is carried out dry-pressing premolding, the 180MPa cold isostatic compaction.
(7) base substrate that moulding is finished places the nitrogen atmosphere stove, and under 1800 ℃ of temperature, sintering 4 hours is product of the present invention.
Embodiment two
(1) takes by weighing BN 50%wt, TiH 225%wt, Al 25%wt, granularity is respectively 1 μ, 2 μ, 2 μ.
(2) in proportion with the powder prepared; Material: alcohol: ball=1: 1.5: 2 (weight), carried out ball mill mixing 12 hours.
(3) material that will mix is crossed 70 mesh sieves 50 ℃ of oven dry 14 hours.
(4) material that will sieve is incubated 6 hours in 1200 ℃ of argon atmospher stoves, carries out chemical reaction.
(5) material that will react carries out ball mill pulverizing again, and oven dry is sieved.
(6) powder that sieves is carried out dry-pressing premolding, the 200MPa cold isostatic compaction.
(7) base substrate that moulding is finished places the nitrogen atmosphere stove, and under 2000 ℃, sintering 2 hours is product of the present invention.
Embodiment three
(1) takes by weighing BN 60%wt, TiH 230%wt, Al 10%wt, granularity is respectively 1 μ, 2 μ, 2 μ.
(2) in proportion with the powder prepared, material: alcohol: ball=1: 1.5: 2 (weight), carried out ball mill mixing 12 hours.
(3) material that will mix is crossed 60 mesh sieves 50 ℃ of oven dry 14 hours.
(4) material that will sieve is incubated 4 hours in 1400 ℃ of argon atmospher stoves, carries out chemical reaction.
(5) material that will react again set by step the condition of (2) carry out ball mill pulverizing, the oven dry, sieve.
(6) powder that sieves is carried out dry-pressing premolding, the 220MPa cold isostatic compaction.
(7) base substrate that moulding is finished places the nitrogen atmosphere stove, and 1900 ℃ of following sintering 3 hours are product of the present invention.

Claims (1)

1, a kind of method of process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter is characterized in that, this method comprises following each step:
(1) be that the following column weight amount of the material powder per-cent of 1~5 μ mixes mutually with granularity:
Silicon nitride: 40~60wt%
Titanium hydride: 20~30wt%
Aluminium powder: 10~30wt%
(2) with the powder of being prepared with weight ratio be: material: alcohol: ball mill mixing is carried out in ball=1: 1.5~2: 2~3, mixing time 10~15 hours;
(3) material that will mix was dried 10~15 hours down at 40~60 ℃, crossed 50~80 mesh standard sieves;
(4) material that will sieve is incubated 4~8 hours in 1000 ℃~1400 ℃ argon gas atmosphere stoves, carries out chemical reaction;
(5) material that will react carries out ball mill pulverizing again, and its ratio of grinding media to material is:
Material: alcohol: ball=1: 1.5~2: 2~3, under 40~60 ℃, dried 10~15 hours, cross 50~80 mesh standard sieves;
(6) material that will sieve gives moldedly, and pressure is 10~20MPa, then cold isostatic compaction under 150~250Mpa;
(7) base substrate that moulding is finished places nitrogen atmosphere, is heated to 1800~2000 ℃, burns 2~5 hours, is ceramic evaporation boat of the present invention.
CN 99119429 1999-09-24 1999-09-24 Process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter method Pending CN1250762A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 99119429 CN1250762A (en) 1999-09-24 1999-09-24 Process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 99119429 CN1250762A (en) 1999-09-24 1999-09-24 Process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter method

Publications (1)

Publication Number Publication Date
CN1250762A true CN1250762A (en) 2000-04-19

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CN 99119429 Pending CN1250762A (en) 1999-09-24 1999-09-24 Process for preparing boron nitride compounded conducting ceramic evaporator by non-pressure sinter method

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100432017C (en) * 2006-07-28 2008-11-12 北京工业大学 Fast prepn process of machinable high-strength SiN-B4C ceramic
CN101928850A (en) * 2010-04-29 2010-12-29 西安理工大学 Method for preparing W-Ti alloy target material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100432017C (en) * 2006-07-28 2008-11-12 北京工业大学 Fast prepn process of machinable high-strength SiN-B4C ceramic
CN101928850A (en) * 2010-04-29 2010-12-29 西安理工大学 Method for preparing W-Ti alloy target material

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