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 PDFInfo
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- 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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- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 8
- 229910052582 BN Inorganic materials 0.000 title claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 230000008020 evaporation Effects 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000005056 compaction Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- -1 Titanium hydride Chemical compound 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 229910000048 titanium hydride Inorganic materials 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000007873 sieving Methods 0.000 abstract 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 1
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000012797 qualification Methods 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- Ceramic Products (AREA)
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
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.
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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ID=5280892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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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| Country | Link |
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| CN (1) | CN1250762A (en) |
Cited By (2)
| 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 |
-
1999
- 1999-09-24 CN CN 99119429 patent/CN1250762A/en active Pending
Cited By (2)
| 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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