CN104775097B - Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method thereof - Google Patents
Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method thereof Download PDFInfo
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- CN104775097B CN104775097B CN201510180484.7A CN201510180484A CN104775097B CN 104775097 B CN104775097 B CN 104775097B CN 201510180484 A CN201510180484 A CN 201510180484A CN 104775097 B CN104775097 B CN 104775097B
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- 229910052796 boron Inorganic materials 0.000 title claims abstract description 43
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 37
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000013077 target material Substances 0.000 title claims abstract description 17
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 238000005507 spraying Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 19
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 238000005488 sandblasting Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000003754 machining Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000010410 layer Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 238000007788 roughening Methods 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910000906 Bronze Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 239000010974 bronze Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000011247 coating layer Substances 0.000 claims description 3
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 238000004513 sizing Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000011521 glass Substances 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000004973 liquid crystal related substance Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 235000013350 formula milk Nutrition 0.000 description 13
- 239000000047 product Substances 0.000 description 10
- 238000001514 detection method Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- 239000007921 spray Substances 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002772 conduction electron Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 235000020610 powder formula Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a low-resistivity micro-boron doped rotary sputtering silicon target material and a preparation method thereof. The target material is prepared from 0.03-0.5wt % of boron and 99.4-99.9wt % of silicon and impurities. The invention also protects the preparation method of the micro-boron doped rotary sputtering silicon target material. According to the invention, by adding boron into silicon in a silicon rotating target material, and introducing a new production process, prepared products are lower in resistivity and high in bonding strength, and the product performance is greatly improved, therefore, the low-resistivity micro-boron doped rotary sputtering silicon target material can be widely applied to the fields of liquid crystal display glass coating, optical coating, and the like, and has a great promoting effect on the progress of industries.
Description
Technical field
The present invention relates to plasma spraying rotary target material field, micro- boron doping rotation of more particularly to a kind of low-resistivity
Sputtering silicon target and preparation method thereof.
Background technology
With the fast development of social economy, electronic product has become during we live indispensable instrument and required
Product.A very crucial part is exactly LCDs in electronic product, while to carry out plated film, glass to LCDs
Plated film is realized by magnetron sputtering membrane process, and the material of the technique is then rotary target material.At present, China and Asia-Pacific
The market demand of regional rotary target material exceedes the 70% of world's aggregate demand, wide market.Magnetron sputtering plating has two
Individual extremely important index parameter, is respectively transmitance and resistivity, and can magnetron sputtering plating index parameter up to standard depend on
The quality of rotary target material, and the quality of rotary target material is determined by its production technology and raw material powder formula.Root is returned to trace to the source,
The problem for affecting the quality of rotary target material most basic is the formula and processing technology of rotary target material.Existing formula is purity
99.9% silicon, remaining is impurity, and production technology is also relatively simple, and the product that this formula and technique are obtained can meet certain
Use requirement, but there is also more obvious defect：Its resistivity is higher, and bond strength is low, should so as to cause client to use
Target production efficiency is relatively low, and abnormality incidence is high, and this will badly influence the fast development of electron trade.
In order to adapt to the demand in market, the problems referred to above in the urgent need to address.
The content of the invention
It is an object of the invention to provide micro- boron sputtering rotation silicon target that a kind of resistivity is low, bond strength is high.
For achieving the above object, the present invention provides a kind of low-resistivity micro- boron doping rotatable sputtering silicon target, and its feature exists
In, being prepared by each composition of following percentage by weight, the boron of 0.03%-0.5%, the silicon of 99.4%-99.9%, remainder is
Impurity is constituted.
Embodiments in accordance with the present invention, there is provided prepared by each composition of following percentage by weight, 0.1% boron,
99.8% silicon, it is remaining for impurity composition.
Embodiments in accordance with the present invention, the micro- boron of the low-resistivity adulterates the preparation method of rotatable sputtering silicon target, and it is special
Levy and be, step is,
1) prepared by rustless steel penstock：
Blanking：The stainless steel tube of fetching measured length is sawed with sawing machine, the internal diameter of steel pipe is 125mm, and external diameter is 133mm；
Che Guan：By stainless steel tube two ends, by product drawing, respectively car goes out groove, oblique angle；
Surface sand-blasting is roughened：Again stainless steel tube is passed through into sandblasting machine by its surface sand-blasting process；
Bottoming：The stainless steel tube after roughening is taken out, by arc-spraying machine, in one layer of bronze aluminium wire material of its surface spraying
Layer, coating layer thickness is 0.5mm, obtains the rustless steel penstock for preparing；
2) prepared by boracic Si powder
Melting：After by a certain percentage silica flour and boron powder mix, high melt is carried out, be smelted into silicon boron ingot.
Broken ball milling：Taking the silicon boron ingot after molding carries out Mechanical Crushing, ball milling, sieves, and prepares the silicon boron of 45-150um
Melting powder；
Drying：The silicon boron melting powder of gained is placed in drying oven and is dried into silicon boron powder material；
Vacuum plasma spray coating：Under vacuum conditions, the use of plasma is that thermal source heats gained silicon boron powder material
To melting or semi-molten state, simultaneously high speed impact, to the rustless steel penstock surface for preparing, forms fine and close silicon boron target coating；Spray
It is 2800-3200L/H that voltage 75-85V, spraying current 550-600A, vacuum are applied for -0.03--0.04Mpa, argon flow amount；
Machining：After vacuum plasma spray coating gained target reaches institute's sizing, the rotary target material of molding is carried out
Machining and electric machining, are cleaned again after completion of processing, are dried.
Embodiments in accordance with the present invention, sand-blast material is the brown firm of 80 mesh for particle diameter in the surface sand-blasting roughening step
Jade, blast time is 1h.
Embodiments in accordance with the present invention, the mixing time of the mixed powder step is 5-6 hours.
Embodiments in accordance with the present invention, the drying temperature in prepared by 3) micro- borosilicate coating is 100 degree, and drying time is
30min。
Embodiments in accordance with the present invention, in the vacuum plasma spray coating step, spray voltage 80V, spraying circuit 550A,
Vacuum is -0.1Mpa, plasma gass flow is 3000L/H.
Impurity in the present invention, Fe≤400ppm, Al≤350ppm, Ni≤50ppm, Mg≤50ppm, Ca≤50ppm, Cu
≤50ppm。
If impurity is a kind of element -- the acceptor impurity in periodic chart in the IIIth race, such as boron or indium, their valency
Electronic band all only has three electronics, and the minimum energy level of their conduction bands less than the conduction electron energy level of the IVth race's element.Cause
This electronics more easily can transit to the conduction band of boron or indium by the valence band of germanium or silicon.In this process, due to losing
Electronics is removed and has generated a cation, because this is " room " for other electronics, generally it has been called
" hole ", and this material is referred to as " P " type quasiconductor.The conduction in such material is mainly caused by the hole of positively charged
, thus in this case electronics is that the impurity that " minority carrier " is mixed is more, the concentration in more sub (hole) is higher, leads
Electrical property is stronger.
The present invention adds boron in the silicon of pure silicon rotary target material material, the recrystallization temperature that can be effectively improved, and reduces again
Crystallization rate, the crystal grain for making silicon target is refined.Boron contents are higher, and the resistivity of target is lower, under identical voltage, pass through
The electric current of target is bigger.Due to power=voltage * electric currents, power can be higher.Such that it is able to improve the magnetron sputtering of client
Film speed, reduces cost.
Generally target is polycrystalline structure, and grain size can be by micron to millimeter magnitude, the target of same composition, fine size
The sputter rate of crystal grain target is faster than coarse grain target；And crystallite dimension differs less target, deposit the thickness distribution of thin film also compared with
Uniformly.Find according to the research of Japanese Energy companies, if the crystallite dimension of silicon target is controlled below 100 μm, and grain size
Change be maintained within 20%, its sputtering gained thin film quality significantly improved.It is demonstrated experimentally that compared with little crystal grain
Target can make sputtering thin film more uniform, and target life is longer, but the sputtering power that to arrange in pairs or groups.
Applicant of the present invention draws suitable addition of the boron in silicon through extremely hard and bitter work, can reach best
Effect.Embodiment 7 compares different boron content, and the resistivity of gained target, crystallite dimension, thickness are equal when other conditions are identical
Even property, sputtering power.It can be seen that under identical spraying coating process, within the specific limits, Boron contents are higher, the resistivity of target is got over
Low, crystallite dimension is less, and client is better with the film thickness uniformity that our target is produced, and client's sputtering power is higher, i.e.,
The production efficiency of client is higher.
Embodiment 1-6 compares different boron content, and the resistivity of the target that different technical parameters are prepared and combination are strong
Degree, it can be seen that when Boron contents addition is definite value, argon flow amount is higher, and bond strength is better, and resistivity is lower；Work as argon
When flow is definite value, Boron contents are higher, and resistivity is lower, and bond strength is poorer.
The present invention adopts the formula of the materials such as B, Si, and introduces new production technology, and the product resistivity for obtaining is lower, and
And transmitance is higher, properties of product are greatly improved, can be widely used for the fields such as LCDs plated film, optical coating, it is right
The progress of industry has great impetus.
Specific embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is intended to for explaining the present invention, and can not
It is interpreted as limitation of the present invention.Unreceipted particular technique or condition person in embodiment, according to described by document in the art
Technology or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being to lead to
Cross city available from conventional products.
Embodiment 1：The preparation of micro- boron doping rotatable sputtering silicon target
Formula composition is shown in Table 1.
The formula composition of each embodiment of table 1 and parameter list
Preparation method：
1. prepared by rustless steel penstock includes following four steps：
1.1) blanking：304 stainless steel tubes of fetching measured length are sawed with sawing machine, the internal diameter of steel pipe is 125mm, and external diameter is
133mm；
1.2) car pipe：By stainless steel tube two ends, by product requirement, respectively car goes out groove, oblique angle etc.；
1.3) surface coarsening：The stainless steel tube of step 1.2 gained is taken out, by sandblasting machine by its surface sand-blasting process, is sprayed
Sand material material is the Brown Alundum that particle diameter is 80 mesh, and blast time is 1h；
1.4) bottoming：The stainless steel tube after step 1.3 roughening is taken out, by arc-spraying machine, in one layer of its surface spraying
Bronze aluminium wire (aluminum (Al):7.5-9.5%；Copper (Cu):90.5-92.5%) material layer, coating layer thickness is 0.5mm,
2. prepared by boracic Si powder
Melting：After by a certain percentage silica flour and boron powder mix, high melt is carried out, be smelted into silicon boron ingot.
Broken ball milling：Taking the silicon boron ingot after molding carries out Mechanical Crushing, ball milling, sieves, and prepares the silicon of 45um-150um
Boron powder.
Drying：The mixed-powder of step 2.1 gained is placed in drying oven, drying temperature is 100 degree, drying time is
30min；
Vacuum plasma spray coating：Under vacuum conditions, the use of plasma is that thermal source heats gained silicon boron powder material
To melting or semi-molten state and the rustless steel penstock surface obtained by high speed impact to step 1.4, fine and close silicon boron target is formed
Coating, in the every technical parameter in spraying process, spray voltage 80V, spraying current 580A, vacuum are -0.04Mpa, argon
Throughput is 2800L/H.
2.4) machining：After vacuum plasma spray coating gained target reaches institute's sizing, the rotary target material to molding
Machining and electric machining are carried out, cleaned again after completion of processing, dried (100 DEG C of drying temperature, time 1hrs) and packaging
Etc. operation, finished product warehouse-in is completed.
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.The results are shown in Table shown in 1.
Embodiment 2：The preparation of micro- boron doping rotatable sputtering silicon target
Formula composition is shown in Table 1, and with embodiment 1, argon flow amount is shown in Table 1 to preparation method, and other parameters are with embodiment 1.
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.The results are shown in Table shown in 1.
Embodiment 3：The preparation of micro- boron doping rotatable sputtering silicon target
Formula composition is shown in Table 1, and with embodiment 1, argon flow amount is shown in Table 1 to preparation method, and other parameters are with embodiment 1.
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.The results are shown in Table shown in 1.
Embodiment 4：The preparation of micro- boron doping rotatable sputtering silicon target
Formula composition is shown in Table 1, and with embodiment 1, argon flow amount is shown in Table 1 to preparation method, and other parameters are with embodiment 1.
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.The results are shown in Table shown in 1.
Embodiment 5：The preparation of micro- boron doping rotatable sputtering silicon target
Formula composition is shown in Table 1, and with embodiment 1, argon flow amount is shown in Table 1 to preparation method, and other parameters are with embodiment 1.
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.The results are shown in Table shown in 1.
Embodiment 6：The preparation of micro- boron doping rotatable sputtering silicon target
Formula composition is shown in Table 1, and with embodiment 1, argon flow amount is shown in Table 1 to preparation method, and other parameters are with embodiment 1.
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.The results are shown in Table shown in 1.
From embodiment 1-6 can be seen that Boron addition for definite value when, argon flow amount is higher, and bond strength is better, resistivity
It is lower；When argon flow amount is definite value, Boron contents are higher, and resistivity is lower, and bond strength is poorer.
With the increase that boron adds, the resistivity of target can be reduced, but while can reduce the bond strength of target.
Embodiment 7：Impact test of the Boron contents to target
Each group of formula composition is shown in Table 2, and with embodiment 1, parameter is shown in Table 2 to preparation method.Wherein spray voltage 80V, spraying electricity
Stream 550A, argon flow amount are 2800L/H.
The each formula of table 2 is constituted and parameter list
GB/T1410-2006 detection resistance rates.GB/T 8642-2002 detect bond strength.GB/T 6394-2002 survey brilliant
Particle size, sputtering power：The numerical value shown on magnetron sputtering apparatus.
Illustrate that, when spraying coating process is identical, Boron contents more high resistivity is lower, and crystallite dimension is less.
Resistivity is low can be caused to be improved using client's sputtering power of product of the present invention, i.e. the production efficiency of client is carried
It is high.
And the little film thickness uniformity for being conducive to improving the film that client is sputtered out using the target of the present invention of crystallite dimension.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art is in the principle and objective without departing from the present invention
In the case of above-described embodiment can be changed within the scope of the invention, change, replace and modification.
Claims (5)
1. a kind of micro- boron of low-resistivity adulterates rotatable sputtering silicon target, it is characterised in that by each composition of following percentage by weight
Prepare, the boron of 0.03%-0.5%, the silicon of 99.4%-99.9%, it is remaining for impurity composition；
The micro- boron of the low-resistivity adulterates the preparation method of rotatable sputtering silicon target, and its step is,
1) prepared by rustless steel penstock：
Blanking：The stainless steel tube of fetching measured length is sawed with sawing machine, the internal diameter of steel pipe is 125mm, and external diameter is 133mm；
Che Guan：By stainless steel tube two ends, by product drawing, respectively car goes out groove, oblique angle；
Surface sand-blasting is roughened：Again stainless steel tube is passed through into sandblasting machine by its surface sand-blasting process；
Bottoming：The stainless steel tube after roughening is taken out, by arc-spraying machine, in one layer of bronze aluminium wire material layer of its surface spraying,
Coating layer thickness is 0.5mm, obtains the rustless steel penstock for preparing；
2) prepared by boracic Si powder
Melting：After by a certain percentage silica flour and boron powder mix, high melt is carried out, be smelted into silicon boron ingot；
Broken ball milling：Taking the silicon boron ingot after molding carries out Mechanical Crushing, ball milling, sieves, and prepares 45-150 μm of silicon boron melting
Powder；
Drying：The silicon boron melting powder of gained is placed in drying oven and is dried into silicon boron powder material；
Vacuum plasma spray coating：Under vacuum conditions, for thermal source gained silicon boron powder material is heated to melt using plasma
Melt or semi-molten state and high speed impact are to the rustless steel penstock surface for preparing, form fine and close silicon boron target coating；Spraying electricity
Pressure 75-85V, spraying current 550-600A, vacuum are -0.03--0.04Mpa, argon flow amount is 2800-3200L/h；
Machining：After vacuum plasma spray coating gained target reaches institute's sizing, machinery is carried out to the rotary target material of molding
Processing and electric machining, are cleaned again after completion of processing, are dried.
2. the micro- boron of low-resistivity described in claim 1 adulterates rotatable sputtering silicon target, it is characterised in that by following percentage by weight
Each composition prepare, 0.1% boron, 99.8% silicon, remaining is impurity composition.
3. the micro- boron of low-resistivity described in claim 1 adulterates the preparation method of rotatable sputtering silicon target, it is characterised in that the table
Sand-blast material is the Brown Alundum that particle diameter is 80 mesh in face sandblasting roughening step, and blast time is 1h.
4. the micro- boron of low-resistivity described in claim 1 adulterates the preparation method of rotatable sputtering silicon target, it is characterised in that described molten
The time mixed in refining step is 5-6 hours.
5. the micro- boron of low-resistivity described in claim 1 adulterates the preparation method of rotatable sputtering silicon target, it is characterised in that the baking
Drying temperature in dry step is 100 degree, and drying time is 30min.
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| CN201510180484.7A CN104775097B (en) | 2014-09-15 | 2015-04-16 | Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method thereof |
| PCT/CN2015/078581 WO2016041361A1 (en) | 2014-09-15 | 2015-05-08 | Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method therefor |
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| CN105929862A (en) * | 2016-04-13 | 2016-09-07 | 广州市尤特新材料有限公司 | Impurity control method for high-purity rotary target material |
| CN106011758B (en) * | 2016-07-20 | 2018-10-19 | 浙江舒玛新材料有限公司 | A kind of optic communication and magnetic store plated film rare earth-transition metal rotary target material and preparation method thereof |
| CN106567045B (en) * | 2016-10-13 | 2019-04-02 | 法柯特科技（江苏）有限公司 | The preparation method of tubular rotary HIGH-PURITY SILICON sputtering target material |
| 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 |
| CN109267019A (en) * | 2017-07-17 | 2019-01-25 | 宁波江丰电子材料股份有限公司 | Silicon rotary target material and preparation method thereof |
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| CN111118437A (en) * | 2019-12-31 | 2020-05-08 | 广州市尤特新材料有限公司 | Rotary silicon-phosphorus alloy target material and preparation method and application thereof |
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| JP6818964B1 (en) * | 2020-06-01 | 2021-01-27 | 三菱電機株式会社 | Composite substrate, manufacturing method of composite substrate, semiconductor device and manufacturing method of semiconductor device |
| CN113481477A (en) * | 2021-06-21 | 2021-10-08 | 芜湖映日科技股份有限公司 | Preparation method of high-transmittance silicon rotary sputtering target material |
| CN113458722A (en) * | 2021-06-24 | 2021-10-01 | 先导薄膜材料有限公司 | Processing method of silicon-aluminum rotary target material |
| CN114044677B (en) * | 2021-11-04 | 2023-01-31 | 大连理工大学 | Silicon-boron master alloy for sputtering target material and preparation method thereof |
| CN114411140B (en) * | 2022-01-19 | 2024-01-30 | 西部宝德科技股份有限公司 | Preparation method of porous titanium coating |
| CN119121150B (en) * | 2024-11-06 | 2025-02-07 | 深圳众诚达应用材料股份有限公司 | High-boron-doped silicon target material, preparation method thereof and solar cell |
| CN119082688B (en) * | 2024-11-06 | 2025-01-10 | 深圳众诚达应用材料股份有限公司 | Silicon target material with high electric conduction and heat conduction, preparation method thereof and optical element |
| CN119082687B (en) * | 2024-11-06 | 2025-02-07 | 深圳众诚达应用材料股份有限公司 | Silicon target material, preparation method thereof and optical device |
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