CN113136552A - Preparation method of ZnS-doped target material - Google Patents
Preparation method of ZnS-doped target material Download PDFInfo
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- CN113136552A CN113136552A CN202110273556.8A CN202110273556A CN113136552A CN 113136552 A CN113136552 A CN 113136552A CN 202110273556 A CN202110273556 A CN 202110273556A CN 113136552 A CN113136552 A CN 113136552A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of a ZnS-doped target material, which comprises the following steps: (1) mixing silver powder and zinc sulfide powder, ball-milling and sieving; (2) putting the powder obtained in the step (1) into a mould, and putting the mould into a vacuum hot-pressing furnace; (3) pre-pressing; (4) molding: vacuumizing until the vacuum degree is less than 10Pa, heating to 700-1050 ℃, preserving heat for 20-60 min, simultaneously pressurizing at 90-150 MPa for 60-120 min, and cooling to obtain the ZnS target material. The invention improves the conductivity of the HP-ZnS target material by doping the Ag element in the zinc sulfide; the doped ZnS target material prepared by the method has the resistivity<5000 Ω. cm, density>98％g/cm3And can be used for a direct current sputtering method.
Description
Technical Field
The invention relates to a preparation method of a target material, in particular to a preparation method of a ZnS-doped target material.
Background
The ZnS polycrystal as an infrared optical material is widely applied to the fields of air-to-air, air-to-ground and ground-to-air missile hoods, infrared imaging guidance systems, infrared windows and the like. The preparation of zinc sulfide polycrystal mainly comprises a vapor deposition method (CVD-ZnS) and a hot pressing method (HP-ZnS), and compared with the CVD-ZnS, the HP-ZnS has the characteristics of excellent mechanical property and optical property, low manufacturing cost and high manufacturing efficiency.
Sputtering is a process of bombarding the surface of a target with high energy to sputter the target. A method for forming a thin film on a substrate by depositing target atoms or molecules in sputtered particles. ZnS prepared by the hot pressing method has no conductivity and is difficult to use by the sputtering method.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a ZnS-doped target material.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a ZnS-doped target material comprises the following steps:
(1) mixing silver powder and zinc sulfide powder, ball-milling and sieving;
(2) putting the powder obtained in the step (1) into a mould, and putting the mould into a vacuum hot-pressing furnace;
(3) pre-pressing;
(4) molding: vacuumizing to less than 10Pa, heating to 700-1050 ℃, preserving heat for 20-60 min, and simultaneously pressurizing at 90-150 MPa for 60-120 min. And cooling to obtain the ZnS target.
The invention improves the conductivity of the HP-ZnS target material by doping the Ag element in the zinc sulfide, and can be applied to a direct current sputtering method. The doped ZnS target material prepared by the method has the resistivity<5000 Ω. cm, density>98％g/cm3And can be used for a direct current sputtering method. As a preferred embodiment of the preparation method of the doped ZnS target, the silver powder is contained in the target in an amount of 0.05 wt% to 0.3 wt%. The doping amount of the silver powder is controlled to be 0.05 wt% -0.3 wt%, if the doping amount of the silver powder is too small, the resistivity is too large to be used for direct current sputtering, and if the doping amount of the silver powder is too large, the performance of a deposited film is affected. More preferably, the content of the silver powder in the target material is 0.1-0.3 wt%, the target material obtained in the range has lower equipment requirement and wider application range, and the resistivity is less than 5000 omega-cm. The resistivity and the subsequent deposition effect are comprehensively considered. More preferably, the silver powder is contained in the target material in an amount of 0.2 wt%.
As a preferred embodiment of the preparation method of the doped ZnS target material, in the step (1), the step of ball milling specifically comprises: ball-milling for 8-12 hours under zirconium balls with diameters of 30mm, 20mm and 10mm and mixed in a weight ratio of 1:1:1, wherein the ball-material ratio is 2-2.5: 1.
As a preferred embodiment of the preparation method of the doped ZnS target material of the present invention, in the step (1), the sieving is 200 mesh sieving.
As a preferred embodiment of the preparation method of the doped ZnS target, in the step (3), the pre-pressing pressure is 50-80 MPa.
As a preferred embodiment of the preparation method of the doped ZnS target, in the step (4), the temperature rise rate is controlled to be 3-5 ℃/min in the temperature rise process.
As a preferred embodiment of the preparation method of the doped ZnS target, step (4) is followed by a step of performing CNC machining on the target and cutting the target to a required size.
As a preferred embodiment of the preparation method of the doped ZnS target material, in the step (4), the cooling mode is furnace temperature reduction.
As a preferred embodiment of the preparation method of the doped ZnS target material of the present invention, in the step (4), the forming is: vacuumizing to vacuum degree less than 10Pa, heating to 950 deg.C at 5 deg.C/min, maintaining for 30min, and pressurizing at 110MPa for 120 min. The target material prepared under the molding condition has lower resistivity and higher relative density.
The invention has the beneficial effects that: the invention provides a preparation method of a ZnS-doped target material, which improves the conductivity of the HP-ZnS target material by doping Ag element in zinc sulfide; the doped ZnS target material prepared by the method has the density>98％g/cm3And the resistivity is low, so that the method can be used in a direct-current sputtering method.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
In an embodiment of the method for preparing a ZnS-doped target according to the present invention, the method includes the following steps:
(1) mixing materials: preparing zinc sulfide powder doped with 0.2 wt% of Ag, and adding the powder with the diameter phi of 30: phi 20: ball-milling zirconium balls with the diameter of 10mm being 1:1:1 for 8 hours in the ball-material ratio of 2.2:1, and sieving the zirconium balls with a 200-mesh sieve;
(2) putting the powder obtained in the step (1) into a high-temperature alloy die, and then putting the die into a vacuum hot-pressing furnace;
(3) pre-pressing: starting cold pre-pressing, wherein the pressurizing pressure is 50 MPa;
(4) molding: vacuumizing to vacuum degree less than 10Pa, heating to 700 deg.C at 3 deg.C/min, maintaining for 20min, and pressurizing at 130MPa for 60 min;
(5) and cooling along with the furnace to obtain a ZnS blank lump material, carrying out CNC machining to obtain the doped ZnS target material, and cutting to a required size according to requirements to obtain a ZnS product.
Example 2
In an embodiment of the method for preparing a ZnS-doped target according to the present invention, the method includes the following steps:
(1) mixing materials: preparing zinc sulfide powder doped with 0.2 wt% of Ag, and adding the powder with the diameter phi of 30: phi 20: ball-milling zirconium balls with the diameter of 10mm being 1:1:1 for 8 hours in the ball-material ratio of 2.2:1, and sieving the zirconium balls with a 200-mesh sieve;
(2) putting the powder obtained in the step (1) into a high-temperature alloy die, and then putting the die into a vacuum hot-pressing furnace;
(3) pre-pressing: starting cold pre-pressing, wherein the pressurizing pressure is 80 MPa;
(4) molding: vacuumizing to vacuum degree less than 10Pa, heating to 950 deg.C at 5 deg.C/min, maintaining for 30min, and pressurizing at 110MPa for 120 min.
(5) And cooling along with the furnace to obtain a ZnS blank lump material, carrying out CNC machining to obtain the doped ZnS target material, and cutting to a required size according to requirements to obtain a ZnS product.
Example 3
In an embodiment of the method for preparing a ZnS-doped target according to the present invention, the method includes the following steps:
(1) mixing materials: preparing zinc sulfide powder doped with 0.2 wt% of Ag, and adding the powder with the diameter phi of 30: phi 20: ball-milling zirconium balls with the diameter of 10mm being 1:1:1 for 8 hours in the ball-material ratio of 2.2:1, and sieving the zirconium balls with a 200-mesh sieve;
(2) putting the powder obtained in the step (1) into a high-temperature alloy die, and then putting the die into a vacuum hot-pressing furnace;
(3) pre-pressing: starting cold pre-pressing, wherein the pressurizing pressure is 80 MPa;
(4) molding: vacuumizing to vacuum degree less than 10Pa, heating to 1050 deg.C at 5 deg.C/min, maintaining for 30min, and pressurizing at 90MPa for 80 min.
(5) And cooling along with the furnace to obtain a ZnS blank lump material, carrying out CNC machining to obtain the doped ZnS target material, and cutting to a required size according to requirements to obtain a ZnS product.
Example 4
In an embodiment of the method for preparing a ZnS-doped target according to the present invention, the method includes the following steps:
(1) mixing materials: preparing zinc sulfide powder doped with 0.2 wt% of Ag, and adding the powder with the diameter phi of 30: phi 20: ball-milling zirconium balls with the diameter of 10mm being 1:1:1 for 8 hours in the ball-material ratio of 2.2:1, and sieving the zirconium balls with a 200-mesh sieve;
(2) putting the powder obtained in the step (1) into a high-temperature alloy die, and then putting the die into a vacuum hot-pressing furnace;
(3) pre-pressing: starting cold pre-pressing, wherein the pressurizing pressure is 50 MPa;
(4) molding: vacuumizing to vacuum degree less than 10Pa, heating to 950 deg.C at 5 deg.C/min, maintaining for 60min, and pressurizing at 150MPa for 60 min.
(5) And cooling along with the furnace to obtain a ZnS blank lump material, carrying out CNC machining to obtain the doped ZnS target material, and cutting to a required size according to requirements to obtain a ZnS product.
Example 5
This example is different from example 2 only in the difference of the molding temperature in step (4), and the temperature in this example is 1050 ℃.
Example 6
The present example is different from example 2 only in the doping amount of the silver powder, and in the present example, the doping amount of the silver powder is 0.05 wt%.
Example 7
The present example is different from example 2 only in the doping amount of the silver powder, and in the present example, the doping amount of the silver powder is 0.1 wt%.
Example 8
The present example is different from example 2 only in the doping amount of the silver powder, and in the present example, the doping amount of the silver powder is 0.3 wt%.
Comparative example 1
This comparative example differs from example 2 only in the difference of the molding temperature in step (4), and the temperature in this comparative example is 1060 ℃. The product obtained by the comparative example has a small amount of decomposition phenomenon and can not meet the use requirement.
Comparative example 2
This comparative example differs from example 2 only in the difference of the molding temperature in step (4), and the temperature in this comparative example is 690 ℃.
Comparative example 3
The comparative example differs from example 2 only in the doping amount of silver powder, which is 0.04 wt% in the comparative example.
The relative density and the resistivity of the targets in the examples 1 to 4 and the comparative example 1 are tested, the relative density is measured by adopting a geometric method, and the resistivity test is carried out by using a four-probe resistivity tester with the model of KDY-1. The test results are shown in Table 1.
TABLE 1
As can be seen from table 1, the zinc sulfide target materials prepared by the preparation methods of examples 1 to 5 have higher relative density and lower resistivity, and the zinc sulfide target materials meeting the requirements cannot be prepared at too high or too low molding temperature, as can be seen from the comparison between examples 2, 6 to 8 and comparative example 3, as the doping amount of Ag increases, the resistivity of the ZnS target material decreases, and when the content of the silver powder in the target material is less than 0.05 wt%, the resistivity is higher, and the silver powder cannot be used in direct current sputtering; when the content of the silver powder in the target material is 0.1-0.3 wt%, the resistivity of the ZnS target material can be lower than 5000 omega-cm, the requirement on equipment is low, and the applicability is high; when the content of the silver powder in the target material is higher than 0.3 wt%, the subsequent deposition effect is affected.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the ZnS-doped target material is characterized by comprising the following steps of:
(1) mixing silver powder and zinc sulfide powder, ball-milling and sieving;
(2) putting the powder obtained in the step (1) into a mould, and putting the mould into a vacuum hot-pressing furnace;
(3) pre-pressing;
(4) molding: vacuumizing until the vacuum degree is less than 10Pa, heating to 700-1050 ℃, preserving heat for 20-60 min, simultaneously pressurizing at 90-150 MPa for 60-120 min, and cooling to obtain the ZnS target material.
2. The method for preparing the doped ZnS target according to claim 1, wherein the silver powder is contained in the target in an amount of 0.05 to 0.3 wt%.
3. The method for preparing the doped ZnS target according to claim 1, wherein the silver powder is contained in the target in an amount of 0.1 to 0.3 wt%.
4. The method for preparing the doped ZnS target according to claim 1, wherein in the step (1), the step of ball milling specifically comprises: ball-milling for 8-12 hours under zirconium balls with diameters of 30mm, 20mm and 10mm and mixed in a weight ratio of 1:1:1, wherein the ball-material ratio is 2-2.5: 1.
5. The method for preparing the doped ZnS target according to claim 1, wherein in the step (1), the sieving is performed by a 200-mesh sieve.
6. The method for preparing the doped ZnS target according to claim 1, wherein in the step (3), the pre-pressing pressure is 50 to 80 MPa.
7. The method for preparing the doped ZnS target according to claim 1, wherein in the step (4), the temperature increase rate is controlled to be 3-5 ℃/min during the temperature increase.
8. The method for preparing a doped ZnS target according to claim 1, wherein the step (4) is followed by a step of CNC machining and cutting the target to a desired size.
9. The method for preparing the doped ZnS target according to claim 1, wherein in the step (4), the cooling is performed by furnace cooling.
10. The method for preparing the doped ZnS target according to claim 1, wherein in the step (4), the forming is: vacuumizing to vacuum degree less than 10Pa, heating to 950 deg.C at 5 deg.C/min, maintaining for 30min, and pressurizing at 110MPa for 120 min.
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| CN202110273556.8A CN113136552A (en) | 2021-03-12 | 2021-03-12 | Preparation method of ZnS-doped target material |
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| CN202110273556.8A CN113136552A (en) | 2021-03-12 | 2021-03-12 | Preparation method of ZnS-doped target material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114804882A (en) * | 2022-05-24 | 2022-07-29 | 先导薄膜材料（广东）有限公司 | Indium selenide doped target material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002373459A (en) * | 2001-06-14 | 2002-12-26 | Sumitomo Metal Mining Co Ltd | Sputtering target for optical disk protecting film, and the optical disk protecting film formed by using the same |
| CN112195446A (en) * | 2020-09-11 | 2021-01-08 | 先导薄膜材料（广东）有限公司 | Arsenic-doped manganous oxide target material and preparation method thereof |
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2021
- 2021-03-12 CN CN202110273556.8A patent/CN113136552A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002373459A (en) * | 2001-06-14 | 2002-12-26 | Sumitomo Metal Mining Co Ltd | Sputtering target for optical disk protecting film, and the optical disk protecting film formed by using the same |
| CN112195446A (en) * | 2020-09-11 | 2021-01-08 | 先导薄膜材料（广东）有限公司 | Arsenic-doped manganous oxide target material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114804882A (en) * | 2022-05-24 | 2022-07-29 | 先导薄膜材料（广东）有限公司 | Indium selenide doped target material and preparation method thereof |
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Application publication date: 20210720 |