CN110835272A - Preparation method of split type conductive ceramic boat - Google Patents
Preparation method of split type conductive ceramic boat Download PDFInfo
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- CN110835272A CN110835272A CN201911233537.1A CN201911233537A CN110835272A CN 110835272 A CN110835272 A CN 110835272A CN 201911233537 A CN201911233537 A CN 201911233537A CN 110835272 A CN110835272 A CN 110835272A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5062—Borides, Nitrides or Silicides
- C04B41/5064—Boron nitride
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Resistance Heating (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a preparation method of a split type conductive ceramic boat, which belongs to the technical field of heater preparation, and the method comprises the steps of machining a graphite heater and the graphite ceramic boat, wherein the graphite heater is a cuboid, the middle part of the graphite heater is a continuous folded lath, the tops of two ends of the graphite heater are provided with U-shaped bosses, U-shaped openings of the two U-shaped bosses are oppositely arranged, a fixing rod is arranged between two ends of the bottom of the graphite heater, the graphite ceramic boat is a cuboid plate, the upper part of the graphite heater is provided with a groove, the outline of the bottom of the graphite ceramic boat is consistent with the outline of the graphite heater, a PBN coating is respectively deposited on the graphite heater except the two ends and the surface of the graphite ceramic boat, and the graphite ceramic boat with the PBN coating is placed on the graphite heater with. The ceramic boat prepared by the method can increase the resistance of the heating part of the ceramic boat, thereby increasing the heating stability of the ceramic boat and prolonging the service life of the conductive ceramic boat.
Description
Technical Field
The invention relates to a preparation method of a split type conductive ceramic boat, in particular to a ceramic boat for metal thermal evaporation, and belongs to the technical field of heaters.
Background
At present at the many electrically conductive ceramic boats that use the graphite material in the metal thermal evaporation field, electrically conductive ceramic boat self can heat and let the metal melt and carry out the evaporation, this process needs carry out mains voltage's adjustment according to the condition that the metal melts and evaporate, electrically conductive ceramic boat of graphite material is because resistance is little now, mains voltage's adjustment is very big to the stability influence that the metal melted and evaporated, electrically conductive ceramic boat damages very easily at this in-process, still need install the adjustment again after the damage, greatly influence the efficiency of scale metal evaporation, the event needs to seek an other solution and realizes the extension of electrically conductive ceramic boat life-span, and reduction in production cost simultaneously.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the split type conductive ceramic boat, and the conductive ceramic boat prepared by the method can obviously prolong the service life of the ceramic boat.
The technical scheme of the invention is as follows:
a preparation method of a split type conductive ceramic boat comprises a graphite heater and the graphite ceramic boat, wherein the graphite heater is a cuboid, the middle part of the graphite heater is a continuous folded batten, U-shaped bosses are arranged on the tops of two ends of the graphite heater respectively, U-shaped openings of the two U-shaped bosses are arranged oppositely, two ends of the graphite heater are connected with a power supply, and a fixing rod is arranged between two ends of the bottom of the graphite heater;
the graphite ceramic boat is a cuboid plate, the upper part of the graphite ceramic boat is provided with a groove, the groove is used for containing molten metal materials, and the outline of the bottom of the graphite ceramic boat is consistent with the outline in the two U-shaped bosses of the graphite heater;
the preparation method comprises the following steps:
(1) machining two ends of the graphite heater, the folding laths, the U-shaped bosses and the fixing rods, wherein the graphite heater is integrally manufactured, and the number of the folding laths is at least two;
(2) adding a PBN protective layer on the graphite heater: coating two ends of the graphite heater in the step (1), putting the graphite heater into a high-temperature reaction furnace, horizontally placing the graphite heater so that the coating of a gap between the folded lines is thicker, introducing gas containing a nitrogen source and a boron source under the conditions that the temperature is 1700-2000 ℃ and the pressure is 10-1000Pa, and depositing a PBN protective layer on the surface of the part of the graphite heater except the two ends;
(3) machining a graphite ceramic boat by a machining mode, wherein the bottom outline of the graphite ceramic boat is matched with the outlines in the two U-shaped bosses of the graphite heater;
(4) adding a PBN coating on the graphite ceramic boat: putting the graphite ceramic boat in the step (3) into a high-temperature reaction furnace, introducing gas containing a nitrogen source and a boron source at the temperature of 1700-2000 ℃ and the pressure of 10-1000Pa, and depositing a PBN coating on the surface of the graphite heater;
(5) the PBN coated graphite ceramic boat was placed on a graphite heater with a PBN protective layer for use.
Preferably, in the step (1), the number of the processed fixing rods is two, the width of the fixing rod is 1-50mm, and the height of the fixing rod is 1-50 mm. The heater is prevented from being deformed.
Preferably, in the step (1), the processed graphite heater has a length of 30-300mm, a width of 10-100mm and a height of 1-50mm, the graphite heater integrally comprises more than two folding strips, the width of the folding strips is 1-50mm, the distance between every two adjacent folding strips is 1-20mm, and U-shaped bosses at two ends of the graphite heater are 1-10mm higher than the middle position of the graphite heater.
Preferably, in the step (1), slope surfaces are processed at the U-shaped openings of the two U-shaped bosses of the graphite heater, and the graphite ceramic boat is gradually compressed from top to bottom when being put in.
Preferably, in the step (2), the PBN protective layer deposited on the surface of the graphite heater has a thickness of 10-500 microns.
Preferably, in the step (3), the graphite ceramic boat has a length of 30-300mm, a width of 10-100mm and a height of 1-30mm, and the groove is 1-20mm lower than the edge position.
Preferably, in the step (4), the thickness of the PBN coating coated on the surface of the graphite ceramic boat is 10-500 microns.
The invention has the beneficial effects that:
the ceramic boat is designed into a heating part and a material-containing melting metal part, the heating part and the material-containing melting metal part are respectively machined and deposited with the protective layers, the graphite heater can be independently designed, and the cross section area of a heater circuit is integrally reduced, so that the resistance of the heating part of the ceramic boat is increased, the heating stability of the ceramic boat is improved, and the service life of the conductive ceramic boat is prolonged.
Drawings
FIG. 1 is a schematic diagram of a graphite heater configuration;
FIG. 2 is a schematic view of a graphite ceramic boat;
FIG. 3 is a schematic structural view of a split type conductive ceramic boat finally obtained by the present invention;
wherein: 1. graphite heater, 2, graphite ceramic boat, 3, the lath that turns back, 4, U type boss, 5, recess, 6, dead lever.
Detailed Description
The present invention will be further described by way of examples, but not limited thereto, with reference to the accompanying drawings.
Example 1:
a preparation method of a split type conductive ceramic boat comprises a graphite heater and the graphite ceramic boat, wherein the graphite heater is a cuboid, the middle part of the graphite heater is a continuous folded batten, U-shaped bosses are arranged on the tops of two ends of the graphite heater respectively, U-shaped openings of the two U-shaped bosses are arranged oppositely, two ends of the graphite heater are connected with a power supply, and a fixing rod is arranged between two ends of the bottom of the graphite heater;
the graphite ceramic boat is a cuboid plate, the upper part of the graphite ceramic boat is provided with a groove, the groove is used for containing molten metal materials, and the outline of the bottom of the graphite ceramic boat is consistent with the outline in the two U-shaped bosses of the graphite heater;
the preparation method comprises the following steps:
(1) the graphite heater is integrally manufactured by machining or other machining modes, the two ends of the graphite heater are folded strips, U-shaped bosses and fixing rods, the graphite heater is 200mm long, 50mm wide and 20mm high, the two ends of the graphite heater are connected with a power supply, the graphite heater integrally comprises 20 folded strips, the folded strips are long strips, the width of each folded strip is 8mm, the distance between every two adjacent folded strips is 2mm, the two ends of the graphite heater are 2mm higher than the middle position, the shape of each folded strip is consistent with the bottom of the graphite ceramic boat, and the graphite ceramic boat can be placed conveniently. The quantity of graphite material dead lever of processing is two, and the length of dead lever is 200mm, and the width is 10mm, highly is 10mm, prevents that the heater from warping.
(2) Adding a PBN protective layer on the graphite heater: and (2) coating two ends of the graphite heater in the step (1), putting the graphite heater into a high-temperature reaction furnace, introducing gas containing a nitrogen source and a boron source at the temperature of 1800 ℃ and under the pressure of 100Pa, and depositing a PBN protective layer with the thickness of 100 microns on the surface of the graphite heater except the two ends.
(3) The graphite ceramic boat is processed by a mechanical or other processing mode, the whole graphite ceramic boat is in a cuboid shape, the length of the graphite ceramic boat is 200mm, the width of the graphite ceramic boat is 50mm, the height of the graphite ceramic boat is 10mm, and the middle position of the graphite ceramic boat is 5mm lower than the edge position of the graphite ceramic boat.
(4) Adding a PBN coating on the graphite ceramic boat: and (3) putting the graphite ceramic boat in the step (3) into a high-temperature reaction furnace, introducing gas containing a nitrogen source and a boron source at 1700 ℃ and 200Pa, and depositing a PBN coating with the thickness of 50 microns on the surface of a graphite heater.
(5) The PBN coated graphite ceramic boat was placed on a graphite heater with a PBN protective layer for use.
The split type conductive ceramic boat obtained by the preparation method of the embodiment is utilized to obtain the change data of the temperature change rate and the power supply current.
Through experiments, the resistance values and the temperature changes under different power supply currents are shown in the following table 1, and the heating is stable.
TABLE 1 resistance and temperature Change Table
Example 2:
the preparation method of the split type conductive ceramic boat comprises the following steps of 1, wherein in the step (1), the length of the graphite heater is 30mm, the width of the graphite heater is 10mm, the height of the graphite heater is 1mm, two ends of the heater are connected with a power supply, the heater integrally comprises 15 folded battens, the folded battens are in a long strip shape, the width of the folded battens is 1mm, the distance between every two adjacent folded battens is 1mm, U-shaped bosses at two ends of the heater are 1mm higher than the middle position of the graphite heater, the shape of the U-shaped bosses is consistent with that of the bottom of the ceramic boat, and the ceramic boat can be conveniently placed. The width of dead lever is 1mm, and the height is 1 mm.
In the step (2), a PBN protective layer is deposited on the other parts of the graphite heater except the two ends by a chemical vapor deposition method, and the thickness of the protective layer is 10 microns.
In the step (3), the graphite ceramic boat is integrally in a cuboid shape, the length of the graphite ceramic boat is 30mm, the width of the graphite ceramic boat is 10mm, the height of the graphite ceramic boat is 1mm, and the middle position of the graphite ceramic boat is 1mm lower than the edge position of the graphite ceramic boat.
In the step (4), the surface of the graphite ceramic boat is coated with a PBN coating, and the thickness of the coating is 10 microns.
Example 3:
the preparation method of the split type conductive ceramic boat comprises the following steps of 1, wherein in the step (1), the length of the graphite heater is 300mm, the width of the graphite heater is 100mm, and the height of the graphite heater is 50mm, the two ends of the heater are connected with a power supply, the heater integrally comprises 5 folding-back battens, the folding-back battens are in a long strip shape, the width of the folding-back battens is 50mm, the distance between every two adjacent folding-back battens is 10mm, U-shaped bosses at the two ends of the heater are 10mm higher than the middle position of the graphite heater, the shape of the U-shaped bosses is consistent with the bottom of the ceramic boat, and the ceramic. The width of dead lever is 50mm, and the height is 50 mm.
In the step (2), a PBN protective layer is deposited on the other parts of the graphite heater except the two ends by a chemical vapor deposition method, and the thickness of the protective layer is 500 microns.
In the step (3), the graphite ceramic boat is integrally rectangular, the length of the graphite ceramic boat is 300mm, the width of the graphite ceramic boat is 100mm, the height of the graphite ceramic boat is 50mm, and the middle position of the graphite ceramic boat is 20mm lower than the edge position of the graphite ceramic boat.
In the step (4), the surface of the graphite ceramic boat is coated with a PBN coating, and the thickness of the coating is 500 microns.
Example 4:
a method for preparing a split conductive ceramic boat, which comprises the following steps of (1) processing slope surfaces at U-shaped openings of two U-shaped bosses of a graphite heater, wherein the graphite ceramic boat is gradually compressed from top to bottom when the graphite ceramic boat is put in.
Claims (7)
1. The preparation method of the split type conductive ceramic boat is characterized in that the conductive ceramic boat comprises a graphite heater and a graphite ceramic boat, wherein the graphite heater is a cuboid, the middle part of the graphite heater is a continuous folded batten, U-shaped bosses are arranged at the tops of two ends of the graphite heater respectively, U-shaped openings of the two U-shaped bosses are oppositely arranged, two ends of the graphite heater are connected with a power supply, and a fixing rod is arranged between two ends of the bottom of the graphite heater;
the graphite ceramic boat is a cuboid plate, the upper part of the graphite ceramic boat is provided with a groove, the groove is used for containing molten metal materials, and the outline of the bottom of the graphite ceramic boat is consistent with the outline in the two U-shaped bosses of the graphite heater;
the preparation method comprises the following steps:
(1) machining two ends of the graphite heater, the folding laths, the U-shaped bosses and the fixing rods, wherein the graphite heater is integrally manufactured, and the number of the folding laths is at least two;
(2) adding a PBN protective layer on the graphite heater: coating two ends of the graphite heater in the step (1), putting the graphite heater into a high-temperature reaction furnace, horizontally placing the graphite heater at 1700-;
(3) machining a graphite ceramic boat by a machining mode, wherein the bottom outline of the graphite ceramic boat is matched with the outlines in the two U-shaped bosses of the graphite heater;
(4) adding a PBN coating on the graphite ceramic boat: putting the graphite ceramic boat in the step (3) into a high-temperature reaction furnace, introducing gas containing a nitrogen source and a boron source at the temperature of 1700-2000 ℃ and the pressure of 10-1000Pa, and depositing a PBN coating on the surface of the graphite heater;
(5) the PBN coated graphite ceramic boat was placed on a graphite heater with a PBN protective layer for use.
2. The method for preparing the split type conductive ceramic boat of claim 1, wherein in the step (1), the number of the processed fixing rods is two, the width of the fixing rods is 1-50mm, and the height of the fixing rods is 1-50 mm.
3. The method for preparing the split type conductive ceramic boat of claim 1, wherein in the step (1), the graphite heater is processed to have a length of 30-300mm, a width of 10-100mm and a height of 1-50mm, the graphite heater integrally comprises more than two folded-back strips, the width of the folded-back strips is 1-50mm, the distance between two adjacent folded-back strips is 1-20mm, and U-shaped bosses at both ends of the graphite heater are 1-10mm higher than the middle position of the graphite heater.
4. The method for preparing the split type conductive ceramic boat of claim 1, wherein in the step (1), the inclined slopes are processed on the U-shaped openings of the two U-shaped bosses of the graphite heater, and the graphite ceramic boat is gradually compressed from top to bottom when being put in.
5. The method for preparing split type conductive ceramic boats as claimed in claim 1, wherein in the step (2), the PBN protective layer deposited on the surface of the graphite heater has a thickness of 10-500 μm.
6. The method for preparing the split type conductive ceramic boat according to claim 1, wherein in the step (3), the graphite ceramic boat has a length of 30-300mm, a width of 10-100mm, a height of 1-30mm, and a groove lower than the edge position by 1-20 mm.
7. The method for preparing split type conductive ceramic boats as claimed in claim 1, wherein in the step (4), the PBN coating layer coated on the surface of the graphite ceramic boat has a thickness of 10-500 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911233537.1A CN110835272A (en) | 2019-12-05 | 2019-12-05 | Preparation method of split type conductive ceramic boat |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911233537.1A CN110835272A (en) | 2019-12-05 | 2019-12-05 | Preparation method of split type conductive ceramic boat |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167508A (en) * | 1994-09-28 | 1997-12-10 | 先进陶瓷公司 | High density flash evaporator |
| US20080173638A1 (en) * | 2007-01-21 | 2008-07-24 | John Thomas Mariner | Encapsulated graphite heater and process |
| CN202792948U (en) * | 2012-08-27 | 2013-03-13 | 北京博宇半导体工艺器皿技术有限公司 | Evaporator crucible with pyrolyzed boron nitride protective layers |
| CN102978574A (en) * | 2012-12-12 | 2013-03-20 | 中国科学院长春光学精密机械与物理研究所 | Evaporation boat for depositing metal alumium film through vacuum thermal evaporation |
| CN202873091U (en) * | 2012-08-27 | 2013-04-10 | 北京博宇半导体工艺器皿技术有限公司 | Heater with pyrolysis boron nitride protection layer |
| CN103114268A (en) * | 2013-03-15 | 2013-05-22 | 福州赛瑞特新材料技术开发有限公司 | Bonded type boron nitride-graphite combined evaporation boat and preparation method thereof |
-
2019
- 2019-12-05 CN CN201911233537.1A patent/CN110835272A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167508A (en) * | 1994-09-28 | 1997-12-10 | 先进陶瓷公司 | High density flash evaporator |
| US20080173638A1 (en) * | 2007-01-21 | 2008-07-24 | John Thomas Mariner | Encapsulated graphite heater and process |
| CN202792948U (en) * | 2012-08-27 | 2013-03-13 | 北京博宇半导体工艺器皿技术有限公司 | Evaporator crucible with pyrolyzed boron nitride protective layers |
| CN202873091U (en) * | 2012-08-27 | 2013-04-10 | 北京博宇半导体工艺器皿技术有限公司 | Heater with pyrolysis boron nitride protection layer |
| CN102978574A (en) * | 2012-12-12 | 2013-03-20 | 中国科学院长春光学精密机械与物理研究所 | Evaporation boat for depositing metal alumium film through vacuum thermal evaporation |
| CN103114268A (en) * | 2013-03-15 | 2013-05-22 | 福州赛瑞特新材料技术开发有限公司 | Bonded type boron nitride-graphite combined evaporation boat and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 朱光雪等: "《思维方式：EQ提升的钥匙》", 31 January 2002, 商务印书馆国际有限公司 * |
| 陈文元等: "《非硅MEMS技术及其应用》", 31 March 2015, 上海交通大学出版社 * |
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Application publication date: 20200225 |