CN106676486B - Production method of ultralow-resistance silicon target material - Google Patents
Production method of ultralow-resistance silicon target material Download PDFInfo
- Publication number
- CN106676486B CN106676486B CN201710004519.0A CN201710004519A CN106676486B CN 106676486 B CN106676486 B CN 106676486B CN 201710004519 A CN201710004519 A CN 201710004519A CN 106676486 B CN106676486 B CN 106676486B
- Authority
- CN
- China
- Prior art keywords
- boron
- content
- silicon
- target material
- silicon target
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention relates to the technical field of silicon target production, in particular to a production method of an ultralow-resistance silicon target. The method adopts the high-boron-content master alloy subjected to acid soaking to be doped, and silicon target production is carried out through an efficient ingot casting process. The invention can ensure that the resistivity of the silicon target material is less than 0.01 omega cm, can reach 0.005 omega cm at the lowest, and has the size range of 500mm multiplied by 500mm, the purity of more than 5.5N and the density of more than 99 percent.
Description
Technical Field
The invention relates to the technical field of silicon target production, in particular to a production method of an ultralow-resistance silicon target.
Background
The resistivity is one of important parameters of silicon target products, except special applications, the resistivity of most silicon targets is required to be as low as possible, the resistivity is required to be within the range of 0.1-0.5 omega cm at the beginning of application and gradually reduced to be less than 0.1 omega cm, the current standard resistivity is 0.02-0.04 omega cm, and when the resistivity is reduced to be below 0.01 omega cm, the amount of the added master alloy is exponentially increased, namely, the amount of the added master alloy is increased from dozens of grams to several kilograms.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a production method of an ultralow-resistance silicon target material. The technical scheme adopted by the invention for realizing the purpose is as follows: a production method of an ultra-low resistance silicon target material is characterized by comprising the following steps: adding the high-boron-content master alloy subjected to acid soaking and a silicon material into a quartz crucible together, and carrying out ingot casting to obtain a silicon ingot with the resistivity of less than 0.01 omega cm.
The production method of the ultra-low resistance silicon target specifically comprises the following steps:
the first step is as follows: calculating the content of boron impurities to be doped according to a silicon material resistivity proportioning formula T ═ (M multiplied by n%)/(M + M), and calculating the mass of the high-boron-content master alloy to be added, wherein T is the content of the boron impurities in the target material, M is the mass of the raw material, M is the mass of the high-boron-content master alloy, and n is the proportion of the boron content in the high-boron-content master alloy;
the second step is that: weighing the high-boron-content mother alloy according to the calculation result of the first step, processing the high-boron-content mother alloy into blocks, soaking the blocks by using a mixed solution of hydrochloric acid and hydrofluoric acid, cleaning the blocks by using clean water, and drying the blocks for later use;
the third step: calculating the mass difference of the high-boron-content mother alloy before and after the second step of treatment, and reckoning the content of boron impurities in the high-boron-content mother alloy after the acid treatment according to the formula in the first step;
the fourth step: according to the calculation result in the third step, reckoning the mass of the acid-treated high-boron-content mother alloy which needs to be added according to the method in the first step;
the fifth step: adding the acid-treated high-boron-content master alloy and a silicon material into a quartz crucible together, and performing high-efficiency ingot casting process treatment to obtain a silicon ingot;
and a sixth step: and cutting and processing the part below the top of the silicon ingot according to the required size to obtain a silicon target product with the resistivity less than 0.01 omega cm.
In said first step n is from 8 to 20 and T is from 4 to 140 ppmw.
And in the second step, the master alloy with high boron content is processed into blocks of 1-3 mm.
In the second step, the mixing ratio of the hydrochloric acid to the hydrofluoric acid is (3-5): 1.
in the second step, the soaking time is 1-10h, and the cleaning is carried out for 3-5 times by using clear water.
And in the sixth step, the area of 20-40mm at the top of the silicon ingot cannot be cut.
And the purity of the silicon target product obtained in the sixth step is more than 5.5N, and the density is more than 99%.
The high boron content master alloy is one of a boron simple substance, silicon-aluminum alloy, silicon-iron alloy or other silicon alloys, and the boron content in the high boron content master alloy is 3000-30000 ppmw.
According to the invention, the mother alloy with high boron content after acid soaking is doped, and after an efficient ingot casting process, the resistivity of the silicon target material is less than 0.01 omega cm and can reach 0.005 omega cm at the lowest, the size range can reach 500mm multiplied by 500mm, the purity is greater than 5.5N, and the density is greater than 99%.
Detailed Description
The present invention is further illustrated below, but the present invention is not limited to the specific examples.
Example 1
A production method of an ultralow-resistance silicon target material is characterized in that a high-boron-content master alloy subjected to acid soaking treatment and a silicon material are added into a quartz crucible together, and a silicon ingot with the resistivity of less than 0.01 omega cm is obtained through an ingot casting process, and specifically comprises the following steps:
the first step is as follows: calculating the content of boron impurities to be doped according to a silicon material resistivity proportioning formula T ═ (M multiplied by n%)/(M + M), and calculating the mass of the high-boron-content master alloy to be added, wherein T is the content of the boron impurities in the target material, M is the raw material mass, M is the mass of the high-boron-content master alloy, n is the proportion of the boron content in the high-boron-content master alloy, n is 8, T is 4ppmw, the high-boron-content master alloy is a boron simple substance, and the content of the boron in the high-boron-content master alloy is 30000 ppmw;
the second step is that: weighing the high-boron-content mother alloy according to the calculation result of the first step, processing the high-boron-content mother alloy into blocks of 1mm, soaking the high-boron-content mother alloy in a mixed solution of hydrochloric acid and hydrofluoric acid, wherein the mixing ratio of the hydrochloric acid to the hydrofluoric acid is 3: 1, soaking for 1h, then cleaning for 3 times by using clear water and drying for later use;
the third step: calculating the mass difference of the high-boron-content master alloy before and after the second step of treatment, and reckoning the content of boron impurities in the high-boron-content master alloy after the acid treatment according to the first step formula;
the fourth step: according to the calculation result in the third step, reckoning the mass of the acid-treated high-boron-content mother alloy which needs to be added according to the method in the first step;
the fifth step: adding the acid-treated high-boron-content master alloy and a silicon material into a quartz crucible together, and carrying out high-efficiency ingot casting process, namely carrying out genetic regulation crystal growth process treatment on the master alloy structure to obtain a silicon ingot;
and a sixth step: and cutting the part below the top of the silicon ingot according to the required size, wherein the part 20mm away from the top of the silicon ingot is not cut in the cutting process, so that the silicon target product with the resistivity less than 0.01 omega-cm, the purity more than 5.5N and the density more than 99 percent is obtained.
Example 2
The steps of the production method of the ultra-low resistance silicon target material in the embodiment are the same as those in the embodiment 1, and the different technical parameters are as follows:
1) in the first step n is 14 and T is 72 ppmw; the high boron content master alloy is silicon-aluminum alloy; the boron content in the high boron content master alloy was 16500 ppmw;
2) in the second step, the master alloy with high boron content is processed into 2mm blocks; the mixing ratio of the hydrochloric acid to the hydrofluoric acid is 4: 1; soaking for 5h, and cleaning with clear water for 4 times;
3) and in the sixth step, the area of 30mm at the top of the silicon ingot is not cut in the cutting process.
Example 3
The steps of the production method of the ultra-low resistance silicon target material in the embodiment are the same as those in the embodiment 1, and the different technical parameters are as follows:
1) in the first step n is 20 and T is 140 ppmw; the high boron content master alloy is ferrosilicon; the boron content in the high boron content master alloy is 3000 ppmw;
2) in the second step, the master alloy with high boron content is processed into 3mm blocks; the mixing ratio of the hydrochloric acid to the hydrofluoric acid is 5: 1; soaking for 10h, and cleaning with clear water for 5 times;
3) and in the sixth step, the area of 40mm at the top of the silicon ingot is not cut in the cutting process.
While there have been shown and described what are at present considered to be the fundamental principles of the invention and the principal features thereof, it will be understood by those skilled in the art that the invention is not limited by the foregoing embodiments, which are given by way of illustration of the principles of the invention, but rather are susceptible to various changes and modifications without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (8)
1. A production method of an ultra-low resistance silicon target material is characterized by comprising the following steps: adding the high-boron-content master alloy subjected to acid soaking and a silicon material into a quartz crucible together, and performing an ingot casting process to obtain a silicon ingot with the resistivity of less than 0.01 omega cm;
the method specifically comprises the following steps:
the first step is as follows: calculating the content of boron impurities to be doped according to a silicon material resistivity proportioning formula T ═ (M multiplied by n%)/(M + M), and calculating the mass of the high-boron-content master alloy to be added, wherein T is the content of the boron impurities in the target material, M is the mass of the silicon material, M is the mass of the high-boron-content master alloy, and n is the proportion of the boron content in the high-boron-content master alloy;
the second step is that: weighing the high-boron-content mother alloy according to the calculation result of the first step, processing the high-boron-content mother alloy into blocks, soaking the blocks by using a mixed solution of hydrochloric acid and hydrofluoric acid, cleaning the blocks by using clean water, and drying the blocks for later use;
the third step: calculating the mass difference of the high-boron-content mother alloy before and after the second step of treatment, and reckoning the content of boron impurities in the high-boron-content mother alloy after the acid treatment according to the formula in the first step;
the fourth step: according to the calculation result in the third step, reckoning the mass of the acid-treated high-boron-content mother alloy which needs to be added according to the method in the first step;
the fifth step: adding the acid-treated high-boron-content master alloy and a silicon material into a quartz crucible together, and performing high-efficiency ingot casting process treatment to obtain a silicon ingot;
and a sixth step: and cutting and processing the part below the top of the silicon ingot according to the required size to obtain a silicon target product with the resistivity less than 0.01 omega cm.
2. The method for producing an ultra-low resistance silicon target material as claimed in claim 1, wherein: in said first step n is from 8 to 20 and T is from 4 to 140 ppmw.
3. The method for producing an ultra-low resistance silicon target material as claimed in claim 1, wherein: and in the second step, the master alloy with high boron content is processed into blocks of 1-3 mm.
4. The method for producing an ultra-low resistance silicon target material as claimed in claim 1, wherein: in the second step, the mixing ratio of the hydrochloric acid to the hydrofluoric acid is (3-5): 1.
5. The method for producing an ultra-low resistance silicon target material as claimed in claim 1, wherein: in the second step, the soaking time is 1-10h, and the cleaning is carried out for 3-5 times by using clear water.
6. The method for producing an ultra-low resistance silicon target material as claimed in claim 1, wherein: and in the sixth step, the area of 20-40mm at the top of the silicon ingot cannot be cut.
7. The method for producing an ultra-low resistance silicon target material as claimed in claim 1, wherein: and the purity of the silicon target product obtained in the sixth step is more than 5.5N, and the density is more than 99%.
8. The method for producing an ultra-low resistance silicon target material as claimed in any one of claims 1 to 7, wherein: the high boron content master alloy is one of a boron simple substance, silicon-aluminum alloy, silicon-iron alloy or other silicon alloys, and the boron content in the high boron content master alloy is 3000-30000 ppmw.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710004519.0A CN106676486B (en) | 2017-01-04 | 2017-01-04 | Production method of ultralow-resistance silicon target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710004519.0A CN106676486B (en) | 2017-01-04 | 2017-01-04 | Production method of ultralow-resistance silicon target material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106676486A CN106676486A (en) | 2017-05-17 |
| CN106676486B true CN106676486B (en) | 2021-05-07 |
Family
ID=58848952
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710004519.0A Active CN106676486B (en) | 2017-01-04 | 2017-01-04 | Production method of ultralow-resistance silicon target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106676486B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01162762A (en) * | 1987-12-18 | 1989-06-27 | Tokyo Electron Ltd | Sputtering device |
| CN102181926A (en) * | 2011-04-08 | 2011-09-14 | 光为绿色新能源有限公司 | Polycrystalline silicon ingot doping method and ingot casting equipment for implementing method |
| CN104451564A (en) * | 2014-11-14 | 2015-03-25 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of target material |
| CN104775097A (en) * | 2014-09-15 | 2015-07-15 | 厦门映日新材料科技有限公司 | Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method thereof |
| CN106133186A (en) * | 2014-04-07 | 2016-11-16 | 东曹Smd有限公司 | Boron doped n-type silicon target |
| 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 |
-
2017
- 2017-01-04 CN CN201710004519.0A patent/CN106676486B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01162762A (en) * | 1987-12-18 | 1989-06-27 | Tokyo Electron Ltd | Sputtering device |
| CN102181926A (en) * | 2011-04-08 | 2011-09-14 | 光为绿色新能源有限公司 | Polycrystalline silicon ingot doping method and ingot casting equipment for implementing method |
| CN106133186A (en) * | 2014-04-07 | 2016-11-16 | 东曹Smd有限公司 | Boron doped n-type silicon target |
| CN104775097A (en) * | 2014-09-15 | 2015-07-15 | 厦门映日新材料科技有限公司 | Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method thereof |
| CN104451564A (en) * | 2014-11-14 | 2015-03-25 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of target material |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106676486A (en) | 2017-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5420609B2 (en) | Titanium target for sputtering | |
| CN104946928A (en) | Titanium alloy with easily refined grains and preparing method thereof | |
| WO2012032610A1 (en) | Titanium material | |
| CN103509984A (en) | Ultrahigh strength aluminum lithium alloy and preparation method thereof | |
| Xie et al. | Deformation twinning in an Fe-6.5 wt.% Si alloy with columnar grains during intermediate temperature compression | |
| CN111926214A (en) | Free-cutting lead brass bar with excellent cold machining plasticity and preparation method thereof | |
| CN102676896A (en) | Corrosion resistant magnesium alloy material and preparation method thereof | |
| CN106521434A (en) | Preparation method of high-purity tantalum target material with preferred orientation | |
| CN106676486B (en) | Production method of ultralow-resistance silicon target material | |
| CN103540877B (en) | A kind of aluminum alloy fin complete processing improving resist collapse performance after soldering | |
| CN102517460A (en) | Method for purifying tantalum powder and tantalum target | |
| CN106048272B (en) | A kind of preparation method of al-mg-si scandium alloy silk | |
| JP2000185999A (en) | Production of alloy single crystal | |
| CN108754248B (en) | Aluminum alloy conductor for overhead stranded wire and manufacturing method thereof | |
| PL403443A1 (en) | Method for producing wires from Cu-Ag alloys | |
| CN101362602A (en) | Purification processing method for drawing casting ingot cleaved bark slat and head material | |
| EP3486340A1 (en) | Aluminum alloy plastic working material and production method therefor | |
| CN106048337A (en) | Method for preparing aluminum alloy wire | |
| CN103938131B (en) | A kind of non-crystaline amorphous metal composition and preparation method | |
| JP5382518B2 (en) | Titanium material | |
| US20120045383A1 (en) | Method for the Manufacture of Photovoltaic Grade Silicon Metal | |
| Yan et al. | Dynamic recrystallization kinetics of as-cast AZ91D alloy | |
| CN102816946A (en) | Copper rod manufacturing process | |
| Deng et al. | Texture evolution in heavily cold-rolled FeCo-2V alloy during annealing | |
| KR101459882B1 (en) | Silicon refining method using metal element |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |