CN104451564A - Preparation method of target material - Google Patents
Preparation method of target material Download PDFInfo
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- CN104451564A CN104451564A CN201410648620.6A CN201410648620A CN104451564A CN 104451564 A CN104451564 A CN 104451564A CN 201410648620 A CN201410648620 A CN 201410648620A CN 104451564 A CN104451564 A CN 104451564A
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- silicon
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- target
- target material
- ingot
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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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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a preparation method of a target material. The method comprises the following steps of mixing and charging a high-purity polycrystalline silicon raw material and a dopant to obtain a mixture, placing the mixture in an ingot furnace, vacuumizing, heating, melting, and carrying out crystal growth, annealing and cooling, cutting and polishing silicon ingots to obtain the square target material. The preparation method is short in production period, the resistivity of the silicon target material can be continuously and accurately controlled by virtue of the amount of the dopant and the silicon target material has the characteristics of uniform distribution, large size, intact crystal and the like.
Description
Technical field
The present invention relates to the preparation field of siliceous target, be specifically related to a kind of method using directional solidification processes to prepare siliceous target.
Technical background
Silicon target is a kind of important sputtering target source, is mainly used in the fields such as glass, display, solar cell, plays a role with the form of silicon fiml or silicon dioxide film.Traditional preparation method is generally powder sintering and crystal pulling method.First silicon material is broken into powder by powder sintering, after being then pressed into target shape, carries out high temperature sintering.The advantage of powder sintering is that silicon target can make default shape, and spillage of material is few, and shortcoming is that silicon target quality prepared by the method is uneven; Crystal pulling method refers to the method adopting single crystal growing, is prepared into silicon single crystal, then enters cutting and is polished to silicon target.
Chinese patent CN101377007A reports a kind of method that crystal pulling method prepares monocrystalline silicon target.Silicon target purity prepared by the method is high, do not have crackle, and be widely used in preparing silicon target material, but silicon target size is less, resistivity regulation range is less, consumes more when making planar targets, limits the application of silicon target in sputtering field.
Summary of the invention
The object of the invention is to overcome the shortcoming and defect that prior art exists, provide a kind of method preparing siliceous target, the method production cycle is fast, and obtained siliceous target has the features such as adjustable, the inner complete and size of resistivity is large.
Technical scheme of the present invention provides a kind of method preparing siliceous target, high-purity polycrystalline silicon raw material is mixed with doping agent after feeding, be placed in ingot furnace vacuumize, heat fused, after long brilliant, annealing and cooling, polishing silicon ingot obtains square target.
According to the method that technique scheme provides, the purity of high-purity polycrystalline silicon raw material is greater than 99.999%, and shape is bulk, particulate state or powder.
According to the method that technique scheme provides, doping agent is selected from least one in pure boron, borosilicate alloy, boron aluminium alloy, and content is for regulating according to resistivity, and after making mixing, the boron concentration of silicon material is 5 ~ 25ppm.
According to the method that technique scheme provides, heat fused process is carried out in two steps, and after first rising to 1560 DEG C with the speed of 260-320 DEG C/h, insulation for some time reheats 0.5h after silicon liquid melts completely.
According to the method that technique scheme provides, long crystalline substance refers to that promoting heat-insulation cage makes the growth velocity of silicon ingot be 1.5cm/h.
According to the method that technique scheme provides, annealing processes 5h at 1360 DEG C.
According to the method that technique scheme provides, cooling refers to that all opening heat-insulation cage to the temperature of silicon ingot is cooled to 200 DEG C.
According to the method that technique scheme provides, the resistivity of obtained siliceous target is 0.025-0.05 Ω cm.
Beneficial effect of the present invention is:
The method that directional solidification processes provided by the invention prepares siliceous target is with short production cycle, and prepared silicon target resistivity accurately controls continuously by the amount of doping agent, and has and be evenly distributed, and target size is large, the features such as crystal perfection.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, the some distortion made and improvement, all belong to protection scope of the present invention.Raw material used in embodiment all can be obtained by commercial sources.
Embodiment 1
130kg silico briquette is evenly placed on bottom quartz crucible, gets the silicon boron alloy of 0.1kg 3%, be divided into 5 heaps and be placed on four corners and central zone respectively, continue 270kg silicon material to add in crucible, silicon is steadily contacted with sidewall of crucible; Crucible is placed in ingot furnace, starts to vacuumize heating, be heated to 1560 DEG C by 5h; Keep 1560 DEG C to continue melted silicon material, after finding that silicon liquid melts completely from view port, then keep 0.5h; (4) slowly promote heat-insulation cage to 17cm, and lower power, keep the silicon ingot speed of growth of 1.5cm/h; After long crystalline substance terminates, at 1360 DEG C, keep 5h to carry out anneal, eliminate internal stress; All open heat-insulation cage, make silicon ingot be quickly cooled to 200 DEG C.Quartz crucible is removed in last blow-on, and polishing silicon ingot surrounding, test resistance rate is about 0.04-0.05 Ω cm.
Embodiment 2
150kg silico briquette is evenly placed on bottom quartz crucible, gets the aluminum silicon alloy of 0.2kg 3%, be divided into 5 heaps and be placed on four corners and central zone respectively, continue 300kg silicon material to add in crucible, silicon is steadily contacted with sidewall of crucible; Crucible is placed in ingot furnace, starts to vacuumize heating, be heated to 1560 DEG C by 6h; Keep 1560 DEG C, continue melted silicon material, after finding that silicon liquid melts completely from view port, then keep 1h; Slow lifting heat-insulation cage to 17cm, and lowers power, keeps the silicon ingot speed of growth of 2cm/h; After long crystalline substance terminates, at 1360 DEG C, keep 5h to carry out anneal, eliminate internal stress; All open heat-insulation cage, make silicon ingot be quickly cooled to 200 DEG C.Quartz crucible is removed in last blow-on, and polishing silicon ingot surrounding, test resistance rate is about 0.025-0.035 Ω cm.
Claims (8)
1. prepare a method for siliceous target, it is characterized in that, high-purity polycrystalline silicon raw material is mixed with doping agent after feeding, be placed in ingot furnace vacuumize, heat fused, after long brilliant, annealing and cooling, cutting polishing silicon ingot obtains square target.
2. preparation method according to claim 1, is characterized in that, the purity of described high-purity polycrystalline silicon raw material is greater than 99.999%, and shape is bulk, particulate state or powder.
3. preparation method according to claim 1, is characterized in that, described doping agent is selected from least one in pure boron, borosilicate alloy, boron aluminium alloy, and regulate the quality of doping agent according to resistivity, after making mixing, the boron concentration of silicon material is 5 ~ 25ppm.
4. preparation method according to claim 1, it is characterized in that, described heat fused process is carried out in two steps, after first rising to 1560 DEG C with the speed of 260-320 DEG C/h, insulation for some time is incubated 0.5-1h again after silicon liquid melts completely, makes silicon liquid uniform composition everywhere.
5. preparation method according to claim 1, is characterized in that, described long crystalline substance refers to that promoting heat-insulation cage makes the growth velocity of silicon ingot be 1-3cm/h.
6. preparation method according to claim 1, is characterized in that, described annealing processes 5h at 1360 DEG C.
7. preparation method according to claim 1, is characterized in that, described cooling refers to that all opening heat-insulation cage to the temperature of silicon ingot is cooled to 200 DEG C.
8. preparation method according to claim 1, is characterized in that, the resistivity of obtained siliceous target is 0.025-0.05 Ω cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410648620.6A CN104451564B (en) | 2014-11-14 | 2014-11-14 | A kind of method preparing siliceous target |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410648620.6A CN104451564B (en) | 2014-11-14 | 2014-11-14 | A kind of method preparing siliceous target |
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| Publication Number | Publication Date |
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| CN104451564A true CN104451564A (en) | 2015-03-25 |
| CN104451564B CN104451564B (en) | 2016-12-07 |
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| CN201410648620.6A Expired - Fee Related CN104451564B (en) | 2014-11-14 | 2014-11-14 | A kind of method preparing siliceous target |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106149050A (en) * | 2016-07-26 | 2016-11-23 | 大连理工大学 | The casting technique of polysilicon target is prepared in a kind of aluminum boron foundry alloy doping |
| CN106245112A (en) * | 2016-08-01 | 2016-12-21 | 大工（青岛）新能源材料技术研究院有限公司 | A kind of casting technique of polysilicon target |
| CN106294302A (en) * | 2016-08-10 | 2017-01-04 | 宁夏高创特能源科技有限公司 | A kind of silicon target dispensing regulation polarity, resistivity measuring method |
| CN106676486A (en) * | 2017-01-04 | 2017-05-17 | 青岛蓝光晶科新材料有限公司 | Production method of ultralow-resistance silicon targets |
| CN109896525A (en) * | 2019-04-04 | 2019-06-18 | 新疆中诚硅材料有限公司 | A kind of preparation method of the high borosilicate powder of high-purity |
| CN114044677A (en) * | 2021-11-04 | 2022-02-15 | 大连理工大学 | Silicon-boron master alloy for sputtering target material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003286565A (en) * | 2002-03-27 | 2003-10-10 | Mitsubishi Materials Corp | Sputtering target and manufacturing method therefor |
| JP2004091819A (en) * | 2002-08-29 | 2004-03-25 | Mitsubishi Materials Corp | Target for sputtering, manufacturing method therefor, and target member |
| CN103422165A (en) * | 2013-07-22 | 2013-12-04 | 湖南红太阳光电科技有限公司 | Polycrystalline silicon and preparation method thereof |
| CN103849931A (en) * | 2014-03-28 | 2014-06-11 | 大连理工大学 | Polycrystalline silicon ingoting process for bottom compensated boron element |
-
2014
- 2014-11-14 CN CN201410648620.6A patent/CN104451564B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003286565A (en) * | 2002-03-27 | 2003-10-10 | Mitsubishi Materials Corp | Sputtering target and manufacturing method therefor |
| JP2004091819A (en) * | 2002-08-29 | 2004-03-25 | Mitsubishi Materials Corp | Target for sputtering, manufacturing method therefor, and target member |
| CN103422165A (en) * | 2013-07-22 | 2013-12-04 | 湖南红太阳光电科技有限公司 | Polycrystalline silicon and preparation method thereof |
| CN103849931A (en) * | 2014-03-28 | 2014-06-11 | 大连理工大学 | Polycrystalline silicon ingoting process for bottom compensated boron element |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106149050A (en) * | 2016-07-26 | 2016-11-23 | 大连理工大学 | The casting technique of polysilicon target is prepared in a kind of aluminum boron foundry alloy doping |
| CN106245112A (en) * | 2016-08-01 | 2016-12-21 | 大工（青岛）新能源材料技术研究院有限公司 | A kind of casting technique of polysilicon target |
| CN106294302A (en) * | 2016-08-10 | 2017-01-04 | 宁夏高创特能源科技有限公司 | A kind of silicon target dispensing regulation polarity, resistivity measuring method |
| CN106294302B (en) * | 2016-08-10 | 2018-10-09 | 宁夏高创特能源科技有限公司 | A kind of silicon target dispensing adjusts polarity, resistivity measuring method |
| CN106676486A (en) * | 2017-01-04 | 2017-05-17 | 青岛蓝光晶科新材料有限公司 | Production method of ultralow-resistance silicon targets |
| CN106676486B (en) * | 2017-01-04 | 2021-05-07 | 青岛蓝光晶科新材料有限公司 | Production method of ultralow-resistance silicon target material |
| CN109896525A (en) * | 2019-04-04 | 2019-06-18 | 新疆中诚硅材料有限公司 | A kind of preparation method of the high borosilicate powder of high-purity |
| CN114044677A (en) * | 2021-11-04 | 2022-02-15 | 大连理工大学 | Silicon-boron master alloy for sputtering target material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN104451564B (en) | 2016-12-07 |
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