CN104775097A - 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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- CN104775097A CN104775097A CN201510180484.7A CN201510180484A CN104775097A CN 104775097 A CN104775097 A CN 104775097A CN 201510180484 A CN201510180484 A CN 201510180484A CN 104775097 A CN104775097 A CN 104775097A
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- 229910052796 boron Inorganic materials 0.000 title claims abstract description 44
- 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
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 29
- 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 24
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 238000005507 spraying Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 22
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims description 19
- 229910001220 stainless steel Inorganic materials 0.000 claims description 19
- 239000010935 stainless steel Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000005488 sandblasting Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 229910000906 Bronze Inorganic materials 0.000 claims description 3
- 229910000831 Steel Inorganic materials 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 3
- 239000010974 bronze Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000004140 cleaning Methods 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
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007788 roughening Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- 235000013350 formula milk Nutrition 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 239000010408 film Substances 0.000 description 8
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- 238000005516 engineering process Methods 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
- 238000007747 plating Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 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
- 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
- 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
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 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
- 239000012528 membrane Substances 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
- 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
- 239000010409 thin film 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 rotatable sputtering silicon target particularly relating to a kind of low-resistivity and preparation method thereof.
Background technology
Along with socioeconomic fast development, electronic product has become indispensable instrument and requisite in our life.In electronic product, very crucial parts are exactly liquid crystal display, and will carry out plated film to liquid crystal display, glass coating is realized by magnetron sputtering membrane process simultaneously, and the material of this technique is then rotary target material.At present, the market demand of China and Asian-Pacific area rotary target material exceedes 70% of world's aggregate demand, wide market.Magnetron sputtering plating has two extremely important index parameters, be through rate and resistivity respectively, can magnetron sputtering plating index parameter up to standardly depend on the quality of rotary target material, and the quality of rotary target material is determined by its production technique and raw material powder formula.Return root to trace to the source, affect the formula and processing technology that the most basic problem of the quality of rotary target material is rotary target material.Existing formula is purity 99.9% silicon, all the other are impurity, production technique is also comparatively simple, the product that this composition and engineering obtains can meet certain service requirements, but also there is comparatively significantly defect: its resistivity is higher, and bonding strength is low, thus causes client to use this target production efficiency lower, 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.
Summary of the invention
Micro-boron sputtering that a kind of resistivity is low, bonding strength is high is the object of the present invention is to provide to rotate silicon target.
For achieving the above object, the invention provides a kind of low-resistivity micro-boron doping rotatable sputtering silicon target, it is characterized in that, prepared by each composition of following weight percent, the boron of 0.03%-0.5%, the silicon of 99.4%-99.9%, remaining is impurity composition.
According to embodiments of the invention, provide and prepared by each composition of following weight percent, the boron of 0.1%, the silicon of 99.8%, remaining is impurity composition.
According to embodiments of the invention, the preparation method of described low-resistivity micro-boron doping rotatable sputtering silicon target, it is characterized in that, step is,
1) stainless steel penstock preparation:
Blanking: with the stainless steel tube of sawing machine saw fetching measured length, 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 go out groove, oblique angle;
Surface sand-blasting alligatoring: again by stainless steel tube by sandblast machine by its surface sand-blasting process;
Bottoming: take out the stainless steel tube after alligatoring, by arc-spraying machine, at its surface spraying one deck bronze aluminium wire material layer, coat-thickness is 0.5mm, obtains the stainless steel penstock prepared;
2) boracic Si powder preparation
Melting: after silica flour and boron powder mix by a certain percentage, carry out high melt, be smelted into silicon boron ingot.
Broken ball milling: get shaping after silicon boron ingot carry out Mechanical Crushing, ball milling, sieve, prepare the silicon boron melting powder of 45-150um;
Dry: the silicon boron melting powder of gained is placed in stoving oven and is dried into silicon boron powder material;
Vacuum plasma spray coating: under vacuum conditions, use plasma body for thermal source by gained silicon boron powder heating materials to melting or semi-melting state and high speed impact is surperficial to the stainless steel penstock for preparing, form fine and close silicon boron target coating; Spray voltage 75-85V, spraying current 550-600A, vacuum tightness are-0.03--0.04Mpa, argon flow amount is 2800-3200L/H;
Mechanical workout: arrive after institute's dimensioning until vacuum plasma spray coating gained target, mechanical workout and electromachining are carried out to shaping rotary target material, carries out again after completion of processing cleaning, drying.
According to embodiments of the invention, in described surface sand-blasting roughening step, sand-blast material is particle diameter is 80 object Brown Alundum, and blast time is 1h.
According to embodiments of the invention, the mixing time of described mixed powder step is 5-6 hour.
According to embodiments of the invention, described 3) bake out temperature in micro-borosilicate coating preparation is 100 degree, and drying time is 30min.
According to embodiments of the invention, in described vacuum plasma spray coating step, spray voltage 80V, spraying circuit 550A, vacuum tightness are-0.1Mpa, plasma gas flow is 3000L/H.
Impurity in the present invention, Fe≤400ppm, Al≤350ppm, Ni≤50ppm, Mg≤50ppm, Ca≤50ppm, Cu≤50ppm.
Such as, if impurity is a kind of element--the acceptor impurity in periodictable in the IIIth race, boron or indium, their valence band all only has three electronics, and the minimum energy level of their conduction bands is lower than the conduction electron energy level of the IVth race's element.Therefore electronics more easily can be transitted to the conduction band of boron or indium by the valence band of germanium or silicon.In this process, create a positive ion owing to losing electronics, because this is " room " for other electronics, so usually it is called in " hole ", and this material is called as " P " N-type semiconductorN.Conduct in such material and mainly caused by the hole of positively charged, thus electronics is that the impurity that " minority carrier " mixes is more in this case, and the concentration of many sons (hole) is higher, and conductivity is stronger.
The present invention adds boron in the silicon of pure silicon rotary target material material, the recrystallization temperature that can effectively improve, and reduces recrystallize speed, makes the crystal grain of silicon target obtain refinement.Boron contents is higher, and the resistivity of target is lower, in same electrical pressure, larger by the electric current of target.Due to power=voltage * electric current, power can be higher.Thus the magnetron sputtering plating speed of client can be improved, reduce costs.
Usual target is polycrystalline structure, and grain size can by micron to millimeter magnitude, the target of same composition, and the sputter rate of fine size crystal grain target is faster than coarse grain target; And the target that grain-size difference is less, the thickness distribution of deposition film is also more even.Find according to the research of Japanese Energy company, if the grain-size of silicon target controlled below 100 μm, and the change of grain size remains within 20%, and the quality of its sputtering gained film can significantly be improved.Experiment proves, the target of less crystal grain can make sputtering thin film comparatively even, and target life is longer, but sputtering power of will arranging in pairs or groups.
Applicant of the present invention, through extremely hard and bitter work, draws the suitable addition of boron in silicon, can reach best effect.Embodiment 7 compares different boron content, resistivity, grain-size, film uniformity, the sputtering power of gained target when other condition is identical.Can find out that, under identical spraying coating process, within the specific limits, Boron contents is higher, the resistivity of target is lower, and grain-size is less, and the film uniformity that client produces with our target is better, and client's sputtering power is higher, and namely the production efficiency of client is higher.
Embodiment 1-6 compares different boron content, the resistivity of the target that different technical parameters prepares and bonding strength, and can find out that argon flow amount is higher when Boron contents addition is definite value, bonding strength is better, and resistivity is lower; When argon flow amount is definite value, Boron contents is higher, and resistivity is lower, and bonding strength is poorer.
The present invention adopts the formula of the materials such as B, Si, and introduces new production technique, and the product resistivity obtained is lower, and transmitance is higher, greatly improve product performance, the fields such as liquid crystal display plated film, optical coating can be widely used in, have great pushing effect to the progress of industry.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
Embodiment 1: the preparation of micro-boron doping rotatable sputtering silicon target
Formula composition is in table 1.
The formula composition of each embodiment of table 1 and parameter list
Preparation method:
1. the preparation of stainless steel penstock comprises following four steps:
1.1) blanking: with 304 stainless steel tubes of sawing machine saw fetching measured length, 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 go out groove, oblique angle etc.;
1.3) surface coarsening: the stainless steel tube taking out step 1.2 gained, by sandblast machine by its surface sand-blasting process, sand-blast material is particle diameter is 80 object Brown Alundum, and blast time is 1h;
1.4) bottoming: take out the stainless steel tube after step 1.3 alligatoring, by arc-spraying machine, at its surface spraying one deck bronze aluminium wire (aluminium (Al): 7.5-9.5%; Copper (Cu): 90.5-92.5%) material layer, coat-thickness is 0.5mm,
2. boracic Si powder preparation
Melting: after silica flour and boron powder mix by a certain percentage, carry out high melt, be smelted into silicon boron ingot.
Broken ball milling: get shaping after silicon boron ingot carry out Mechanical Crushing, ball milling, sieve, prepare the silicon boron powder of 45um-150um.
Dry: the mixed powder of step 2.1 gained is placed in stoving oven, and bake out temperature is 100 degree, and drying time is 30min;
Vacuum plasma spray coating: under vacuum conditions, use plasma body for thermal source by gained silicon boron powder heating materials to melting or semi-melting state and the stainless steel penstock that obtains to step 1.4 of high speed impact is surperficial, form fine and close silicon boron target coating, in every technical parameter in spraying process, spray voltage 80V, spraying current 580A, vacuum tightness are-0.04Mpa, argon flow amount is 2800L/H.
2.4) mechanical workout: arrive after institute's dimensioning until vacuum plasma spray coating gained target, mechanical workout and electromachining are carried out to shaping rotary target material, carry out again after completion of processing cleaning, drying (bake out temperature 100 DEG C, time 1hrs) and the operation such as packaging, namely finished product warehouse-in completes.
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding 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 in table 1, and preparation method is with embodiment 1, and argon flow amount is in table 1, and other parameter is with embodiment 1.
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding 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 in table 1, and preparation method is with embodiment 1, and argon flow amount is in table 1, and other parameter is with embodiment 1.
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding 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 in table 1, and preparation method is with embodiment 1, and argon flow amount is in table 1, and other parameter is with embodiment 1.
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding 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 in table 1, and preparation method is with embodiment 1, and argon flow amount is in table 1, and other parameter is with embodiment 1.
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding 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 in table 1, and preparation method is with embodiment 1, and argon flow amount is in table 1, and other parameter is with embodiment 1.
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding strength.The results are shown in Table shown in 1.
As can be seen from embodiment 1-6, when Boron addition is definite value, argon flow amount is higher, and bonding strength is better, and resistivity is lower; When argon flow amount is definite value, Boron contents is higher, and resistivity is lower, and bonding strength is poorer.
Along with the increase that boron adds, the resistivity of target can reduce, but can reduce the bonding strength of target simultaneously.
Embodiment 7: Boron contents is tested the impact of target
Each group of formula composition is in table 2, and preparation method is with embodiment 1, and parameter is in table 2.Wherein spray voltage 80V, spraying current 550A, argon flow amount are 2800L/H.
Table 2 is formula composition and parameter list respectively
GB/T1410-2006 detects resistivity.GB/T 8642-2002 detects bonding strength.GB/T 6394-2002 surveys grain-size, sputtering power: the numerical value that magnetron sputtering apparatus shows.
Illustrate that, when spraying coating process is identical, Boron contents more high resistivity is lower, and grain-size is less.
The low client's sputtering power using product of the present invention that can make of resistivity improves, and namely the production efficiency of client improves.
And the little film uniformity being conducive to the film that raising client uses target of the present invention to sputter out of grain-size.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (7)
1. low-resistivity micro-boron doping rotatable sputtering silicon target, is characterized in that, prepared by each composition of following weight percent, the boron of 0.03%-0.5%, the silicon of 99.4%-99.9%, and remaining is impurity composition.
2. the micro-boron doping of low-resistivity described in claim 1 rotatable sputtering silicon target, is characterized in that, prepared by each composition of following weight percent, the boron of 0.1%, the silicon of 99.8%, and remaining is impurity composition.
3. a preparation method for the micro-boron doping of low-resistivity described in claim 1 or 2 rotatable sputtering silicon target, it is characterized in that, step is,
1) stainless steel penstock preparation:
Blanking: with the stainless steel tube of sawing machine saw fetching measured length, 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 go out groove, oblique angle;
Surface sand-blasting alligatoring: again by stainless steel tube by sandblast machine by its surface sand-blasting process;
Bottoming: take out the stainless steel tube after alligatoring, by arc-spraying machine, at its surface spraying one deck bronze aluminium wire material layer, coat-thickness is 0.5mm, obtains the stainless steel penstock prepared;
2) boracic Si powder preparation
Melting: after silica flour and boron powder mix by a certain percentage, carry out high melt, be smelted into silicon boron ingot.
Broken ball milling: get shaping after silicon boron ingot carry out Mechanical Crushing, ball milling, sieve, prepare the silicon boron melting powder of 45-150um;
Dry: the silicon boron melting powder of gained is placed in stoving oven and is dried into silicon boron powder material;
Vacuum plasma spray coating: under vacuum conditions, use plasma body for thermal source by gained silicon boron powder heating materials to melting or semi-melting state and high speed impact is surperficial to the stainless steel penstock for preparing, form fine and close silicon boron target coating; Spray voltage 75-85V, spraying current 550-600A, vacuum tightness are-0.03--0.04Mpa, argon flow amount is 2800-3200L/H;
Mechanical workout: arrive after institute's dimensioning until vacuum plasma spray coating gained target, mechanical workout and electromachining are carried out to shaping rotary target material, carries out again after completion of processing cleaning, drying.
4. the preparation method of the micro-boron doping of low-resistivity described in claim 3 rotatable sputtering silicon target, it is characterized in that, in described surface sand-blasting roughening step, sand-blast material is particle diameter is 80 object Brown Alundum, and blast time is 1h.
5. the preparation method of the micro-boron doping of low-resistivity described in claim 3 rotatable sputtering silicon target, it is characterized in that, the mixing time of described mixed powder step is 5-6 hour.
6. the preparation method of the micro-boron of low-resistivity described in claim 3 doping rotatable sputtering silicon target, is characterized in that, described 3) bake out temperature in micro-borosilicate coating preparation is 100 degree, drying time is 30min.
7. the preparation method of the micro-boron doping of low-resistivity described in claim 3 rotatable sputtering silicon target, it is characterized in that, in described vacuum plasma spray coating step, spray voltage 80V, spraying circuit 550A, vacuum tightness are-0.1Mpa, plasma gas flow is 3000L/H.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410465726 | 2014-09-15 | ||
| CN2014104657262 | 2014-09-15 | ||
| CN201510180484.7A CN104775097B (en) | 2014-09-15 | 2015-04-16 | Low-resistivity micro-boron doped rotary sputtering silicon target material and preparation method thereof |
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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 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01162762A (en) * | 1987-12-18 | 1989-06-27 | Tokyo Electron Ltd | Sputtering device |
| JP2003322955A (en) * | 2002-04-26 | 2003-11-14 | Hoya Corp | Method for producing lithography mask blank, lithography mask and halftone phase shifting mask blank |
| CN1525562A (en) * | 2003-02-28 | 2004-09-01 | ��ʽ���綫֥ | Semiconductor device and manufacturing method thereof |
| CN101348894A (en) * | 2007-07-20 | 2009-01-21 | 乐金显示有限公司 | Method of forming inorganic insulating layer and method of fabricating array substrate for display device using the same |
| CN103346069A (en) * | 2013-06-21 | 2013-10-09 | 中国科学院宁波材料技术与工程研究所 | Method for preparing low-boron-doped high-conductivity hydrogenated amorphous silicon film |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2096189A1 (en) * | 2008-02-28 | 2009-09-02 | Applied Materials, Inc. | Sprayed Si- or Si:Al-target with low iron content |
| CN202148348U (en) * | 2011-06-30 | 2012-02-22 | 厦门映日光电科技有限公司 | Rotary target |
| CN103045995B (en) * | 2012-12-19 | 2015-08-05 | 西北稀有金属材料研究院 | A kind of Rotary niobium oxide target material and preparation method thereof |
-
2015
- 2015-04-16 CN CN201510180484.7A patent/CN104775097B/en active Active
- 2015-05-08 WO PCT/CN2015/078581 patent/WO2016041361A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01162762A (en) * | 1987-12-18 | 1989-06-27 | Tokyo Electron Ltd | Sputtering device |
| JP2003322955A (en) * | 2002-04-26 | 2003-11-14 | Hoya Corp | Method for producing lithography mask blank, lithography mask and halftone phase shifting mask blank |
| CN1525562A (en) * | 2003-02-28 | 2004-09-01 | ��ʽ���綫֥ | Semiconductor device and manufacturing method thereof |
| CN101348894A (en) * | 2007-07-20 | 2009-01-21 | 乐金显示有限公司 | Method of forming inorganic insulating layer and method of fabricating array substrate for display device using the same |
| CN103346069A (en) * | 2013-06-21 | 2013-10-09 | 中国科学院宁波材料技术与工程研究所 | Method for preparing low-boron-doped high-conductivity hydrogenated amorphous silicon film |
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| 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 |
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| CN119121150A (en) * | 2024-11-06 | 2024-12-13 | 深圳众诚达应用材料股份有限公司 | A high-boron-doped silicon target material and 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 |
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| CN104775097B (en) | 2017-04-12 |
| WO2016041361A1 (en) | 2016-03-24 |
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