CN117051365A - Hanging firing type large-size rotary target sintering method - Google Patents
Hanging firing type large-size rotary target sintering method Download PDFInfo
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- CN117051365A CN117051365A CN202311020602.9A CN202311020602A CN117051365A CN 117051365 A CN117051365 A CN 117051365A CN 202311020602 A CN202311020602 A CN 202311020602A CN 117051365 A CN117051365 A CN 117051365A
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- 238000005245 sintering Methods 0.000 title claims abstract description 66
- 238000010304 firing Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000013077 target material Substances 0.000 claims abstract description 8
- 238000007781 pre-processing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 230000008719 thickening Effects 0.000 abstract description 3
- 230000005484 gravity Effects 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
Classifications
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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
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
- C04B2235/6585—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage above that of air
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a hanging firing type large-size rotary target sintering method, which belongs to the technical field of target material processing and comprises the following steps: step one, preparing a large-size rotary target blank, wherein the outer diameter of the bottom of the blank is larger than that of a rotary target main body; step two, pre-sintering the large-size rotary target blank until the density is 85+/-2%; step three, preprocessing the presintered rotary target material, and processing a circular ring step at the bottom of the presintered blank obtained in the step two; and fourthly, placing the prefabricated rotary target on a hanging firing device, placing the rotary target into a sintering furnace for sintering, naturally cooling to room temperature, and ending the sintering. The method reduces the deformation of the bottom opening and the target main body, strengthens the internal and external heat convection of the long rotary target, and ensures uniform heating, thereby ensuring uniform shrinkage of the whole rotary target main body, reducing a series of production costs of materials, processing, recycling, processing and the like caused by thickening and sintering, improving the sintering yield and ensuring the production efficiency.
Description
Technical Field
The invention belongs to the technical field of target processing, and particularly relates to a hanging firing type large-size rotary target sintering method.
Background
With the application and industrial production of ceramic targets, flat Panel Displays (FPDs) have largely replaced the original computer display and television markets, which are mainly Cathode Ray Tubes (CRTs). The technology and market demands of the ITO target material are greatly increased. And the wide application of large-sized flat panel displays, large-sized rotary targets are indispensable.
The problem of shrinkage of the lower bottom opening caused by self gravity and stress in the sintering process of the large-size rotary target is solved, and the common type has a horn mouth caused by uneven shrinkage; and the main body is bent and deformed in the sintering process due to the factors of self gravity sintering heating, uneven atmosphere and the like.
The conventional solution increases the thickness of the rotary target, which increases a series of production costs such as material consumption, processing, recycling, processing and the like, and the yield is difficult to ensure.
Disclosure of Invention
In order to solve the problems in the sintering process of the large-size rotary target, the invention provides a hanging sintering type large-size rotary target sintering method, which comprises the steps of pre-sintering the large-size rotary target, pre-processing the pre-sintered rotary target, and finally placing the pre-sintered rotary target on a hanging sintering device for sintering. The mode reduces the production cost of the large-size rotary target and ensures the yield of target production.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a hanging firing type large-size rotary target sintering method comprises the following steps:
step one, preparing a large-size rotary target blank, wherein the outer diameter of the bottom of the blank is larger than that of a rotary target main body;
step two, pre-sintering the large-size rotary target blank until the density is 85% +/-2%;
step three, preprocessing the presintered rotary target material, and processing a circular ring step at the bottom of the presintered blank obtained in the step two;
and fourthly, placing the prefabricated rotary target on a hanging firing device, placing the rotary target into a sintering furnace for sintering, naturally cooling to room temperature, and ending the sintering.
The technical scheme of the invention is further improved as follows: the annular width of the annular step in the second step is 10-15mm, and the thickness is 6-10mm.
The technical scheme of the invention is further improved as follows: the large-size rotary target size is larger than 700mm, and the large-size rotary target blank is prepared by adopting a conical head rotary target die.
The technical scheme of the invention is further improved as follows: in the first step, the sintering temperature of the rotary target blank is 1350-1450 ℃, the heat preservation is carried out for 2-5h, the equipment used for presintering is a normal temperature and pressure furnace, and the sintering atmosphere is oxygen.
The technical scheme of the invention is further improved as follows: the hanging burning device comprises a burning bearing plate, wherein a clamping interface is arranged in the middle of the burning bearing plate, the clamping interface is an inverted circular truncated cone-shaped opening, the minimum inner diameter of the clamping interface is larger than the outer diameter of the rotary target main body, and the maximum inner diameter of the clamping interface is smaller than the outer diameter of the circular ring step.
The technical scheme of the invention is further improved as follows: the prefabricated rotary target material passes through the clamping interface of the burning-bearing plate, the annular step is clamped at the clamping interface, the burning-bearing plate is hoisted and sintered, and the rotary target is ensured to be vertical to the horizontal plane.
The technical scheme of the invention is further improved as follows: the inclined wall of the clamping interface forms an inclined angle of 15-30 degrees with the horizontal plane.
The technical scheme of the invention is further improved as follows: and step four, sintering the rotary target in a sintering furnace at 1550-1600 ℃ for 5-10h.
By adopting the technical scheme, the invention has the following technical progress:
the invention adopts a hanging firing type large-size rotary target sintering mode, reduces the deformation of the bottom opening and the target main body, strengthens the internal and external heat convection of the long rotary target and ensures uniform heating. Thereby guaranteeing the uniform shrinkage of the whole rotary target main body, reducing a series of production costs such as materials, processing, recycling, processing and the like caused by thickening and sintering, improving the sintering yield and guaranteeing the production efficiency.
Drawings
FIG. 1 is a schematic illustration of a rotary target after pre-processing in accordance with the present invention;
FIG. 2 is a schematic view of a hanging firing device according to the present invention;
FIG. 3 is a schematic diagram of a card interface;
FIG. 4 is a schematic view of the rotary target of the present invention after being placed in a firing device;
wherein, 1, ring step, 2, rotatory target main part, 3, the burning plate, 4, the joint, a, ring step external diameter, b, ring step thickness.
Detailed Description
The invention is further illustrated by the following examples:
the embodiment provides a sintering method of a large-size rotary target, which comprises the following steps:
preparing a large-size rotary target blank by using a conical head rotary target die, wherein the outer diameter of the blank at the bottom is larger than the outer diameter of a rotary target blank main body;
presintering the large-size rotary target blank, placing the blank in a normal temperature and pressure furnace, and preserving heat for 2 hours at the sintering temperature of 1400 ℃ in an oxygen atmosphere to obtain a presintered blank target;
step three, pre-processing the presintered target, carrying out conical chamfering on the bottom of the blank target, and processing the conical position into a circular ring step 1, wherein the circular ring width of the circular ring step is 10-15mm and the thickness is 6-10mm as shown in fig. 1, and the specific size data of the circular ring step outer diameter a, the circular ring step thickness b and the large-size rotary target in each period in the embodiment are shown in the following table.
And fourthly, placing the prefabricated large-size rotary target on a sintering plate 3, placing the sintering plate into a sintering furnace, clamping the annular step 1 at the clamping interface 4, enabling the rotary target main body 2 to be vertical to the horizontal plane, enabling the bottom of the rotary target to be positioned at a vent position, and ensuring uniform entry of oxygen atmosphere. And heating the sintering furnace to 1580 ℃, preserving heat for 5 hours, and finally waiting for natural cooling to room temperature, and ending sintering.
The inclined wall of the clamping interface 4 and the horizontal plane form an inclined angle alpha of 15-30 degrees, the clamping interface 4 is an inverted circular truncated cone-shaped opening, the minimum inner diameter of the clamping interface 4 is larger than the outer diameter of the rotary target body, and the maximum inner diameter of the clamping interface 4 is smaller than the outer diameter of the circular ring step 1, so that the lower edge of the circular ring step 1 of the rotary target is clamped at the clamping interface 4 of the burning bearing plate 3, and the sintering of the periphery of the circular ring step 1 is not affected.
The specific dimension data of the circular ring step outer diameter a and the circular ring step thickness b and the inner and outer diameters of the large-size rotary target body in each period are shown in the following table:
note that: yield = finished weight/blank weight
The large-size rotary target material after the operation is performed: the bottom port is uniformly contracted, and no flare opening exists; the straightness of the whole rotary target is good. Then large-size rotary targets are manufactured in batches by the technology, curvature measurement and density detection in the vertical directions are carried out, and specific data are as follows: (Unit: mm/m)
Bending: | 0.3 | 0.4 | 0.3 | 0.2 | 0.1 | 0.2 | 0.1 | 0.2 |
comparative example 1
In the prior art, a large-size rotary target blank is placed on a sintering bearing plate in a vertical horizontal plane, and a certain sintering curve is arranged in an atmosphere sintering furnace to control sintering.
Firstly, preparing a large-size rotary target blank by using a thickening rotary target die. And then placing the thickened large-size rotary target blank in a normal temperature and normal pressure furnace, sintering at the temperature of 1580 ℃ in an oxygen atmosphere, preserving heat for 5 hours, and finally waiting for cooling to the room temperature, and ending sintering.
The large-size rotary target after the above operation:
note that: yield = finished weight/blank weight
The sintering atmosphere is uneven, the temperature is also uneven, the shrinkage of the bottom of the rotary target is uneven under the influence of high temperature, self gravity stress and temperature difference, and the main body has bending deformation to a certain extent.
Therefore, the sintering mode of the embodiment can effectively solve a series of shrinkage problems such as small shrinkage, uneven bell mouth and the like of the bottom mouth in the sintering process of the large-size rotary target, and greatly improves the yield and the good product rate. And the lifting sintering is adopted to strengthen the internal and external heat convection, so that the stability of the density of the whole rotary target is ensured, and the product quality is improved.
Claims (8)
1. A hanging firing type large-size rotary target sintering method is characterized by comprising the following steps:
step one, preparing a large-size rotary target blank, wherein the outer diameter of the bottom of the blank is larger than that of a rotary target main body;
step two, pre-sintering the large-size rotary target blank until the density is 85% +/-2%;
step three, preprocessing the presintered rotary target material, and processing a circular ring step (1) at the bottom of the presintered blank obtained in the step two;
and fourthly, placing the prefabricated rotary target on a hanging firing device, placing the rotary target into a sintering furnace for sintering, naturally cooling to room temperature, and ending the sintering.
2. The hanging firing type large-size rotary target sintering method according to claim 1, characterized in that: the annular width of the annular step in the second step is 10-15mm, and the thickness is 6-10mm.
3. The hanging firing type large-size rotary target sintering method according to claim 1, characterized in that: the large-size rotary target size is larger than 700mm, and the large-size rotary target blank is prepared by adopting a conical head rotary target die.
4. The hanging firing type large-size rotary target sintering method according to claim 1, characterized in that: in the first step, the sintering temperature of the rotary target blank is 1350-1450 ℃, the heat preservation is carried out for 2-5h, the equipment used for presintering is a normal temperature and pressure furnace, and the sintering atmosphere is oxygen.
5. The hanging firing type large-size rotary target sintering method according to claim 1, characterized in that: the hanging firing device comprises a firing plate (3) with a clamping interface (4) arranged in the middle, the clamping interface (4) is an inverted circular truncated cone-shaped opening, the minimum inner diameter of the clamping interface (4) is larger than the outer diameter of a rotary target main body, and the maximum inner diameter of the clamping interface (4) is smaller than the outer diameter of the circular ring step (1).
6. The hanging firing type large-size rotary target sintering method according to claim 1, characterized in that: the prefabricated rotary target material passes through the clamping interface (4) of the bearing plate (3), the annular step (1) is clamped at the clamping interface (4), the bearing plate is hung up for sintering, and the rotary target is ensured to be vertical to the horizontal plane.
7. The hanging firing type large-size rotary target sintering method according to claim 5, characterized in that: the inclined wall of the clamping interface (4) forms an inclined angle of 15-30 degrees with the horizontal plane.
8. The hanging firing type large-size rotary target sintering method according to claim 1, characterized in that: and step four, sintering the rotary target in a sintering furnace at 1550-1600 ℃ for 5-10h.
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CN202311020602.9A CN117051365A (en) | 2023-08-15 | 2023-08-15 | Hanging firing type large-size rotary target sintering method |
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CN202311020602.9A CN117051365A (en) | 2023-08-15 | 2023-08-15 | Hanging firing type large-size rotary target sintering method |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115894009A (en) * | 2022-11-14 | 2023-04-04 | 先导薄膜材料(广东)有限公司 | Rapid sintering and degreasing method for ITO (indium tin oxide) planar target and supporting plate used by rapid sintering and degreasing method |
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2023
- 2023-08-15 CN CN202311020602.9A patent/CN117051365A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115894009A (en) * | 2022-11-14 | 2023-04-04 | 先导薄膜材料(广东)有限公司 | Rapid sintering and degreasing method for ITO (indium tin oxide) planar target and supporting plate used by rapid sintering and degreasing method |
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