CN117105649A - Preparation method of silicon oxide evaporation material - Google Patents
Preparation method of silicon oxide evaporation material Download PDFInfo
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- CN117105649A CN117105649A CN202311089964.3A CN202311089964A CN117105649A CN 117105649 A CN117105649 A CN 117105649A CN 202311089964 A CN202311089964 A CN 202311089964A CN 117105649 A CN117105649 A CN 117105649A
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- sintering
- silicon oxide
- evaporation material
- ball milling
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000000463 material Substances 0.000 title claims abstract description 90
- 238000001704 evaporation Methods 0.000 title claims abstract description 72
- 230000008020 evaporation Effects 0.000 title claims abstract description 71
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 60
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 42
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 239000011812 mixed powder Substances 0.000 claims abstract description 16
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000000428 dust Substances 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 239000002893 slag Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000011068 loading method Methods 0.000 description 7
- 238000007740 vapor deposition Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- 239000011364 vaporized material Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- C23C14/10—Glass or silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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Abstract
The invention provides a preparation method of a silicon oxide evaporation material, which comprises the following steps: mixing silica powder with a binder, and performing ball milling to obtain mixed powder; cold isostatic pressing is carried out on the obtained mixed powder to obtain a blank; crushing the obtained blank, and sintering to obtain a sintered material; and classifying and sieving the obtained sintered material to obtain the silicon oxide evaporation material. The silicon oxide evaporation material prepared by the preparation method provided by the invention has high purity and high density, can reach more than 99.0%, has uniform granularity and no slag on the surface, and has stable performance and good evaporation effect when being applied to evaporation.
Description
Technical Field
The invention belongs to the technical field of evaporation coating, and relates to an evaporation material, in particular to a preparation method of a silicon oxide evaporation material.
Background
Vacuum evaporation coating is a technique for obtaining a thin film by evaporating a substance by heating it by an evaporation source under vacuum conditions to deposit it on the surface of a substrate material. The evaporated material is called a vapor deposition material. The vacuum evaporation coating technology has the characteristics of simplicity, convenience, convenient operation, high film forming speed and the like, and is mainly applied to coating of optical components, LEDs, flat panel displays and semiconductor discrete devices. With the rapid development of the optical industry, the performance requirements of the high-end industry on the vapor deposition material are higher and higher, and the quality of the vapor deposition material directly influences the quality of the coating film.
CN104557039a discloses a medium refractive index evaporation coating material, a preparation process and application thereof, the composition of the evaporation coating material comprises lanthanum oxide, aluminum oxide and silicon dioxide, the evaporation coating material is prepared by sequentially carrying out the processes of mixing reaction, compression molding and high-temperature sintering, a single-layer film with a refractive index of 1.75 can be obtained by evaporation, and the stability is good.
CN107285753a discloses a preparation method of a low refractive index evaporation material, which comprises the following steps: siO is made of 2 And Al 2 O 3 The preparation method comprises the steps of proportioning, ball milling, slurry drying, tabletting, forming, sintering and cleaning, and the prepared evaporation material has the advantages of no splashing, high density and stable evaporation rate when used for coating.
CN115893992a discloses a method for preparing silicon oxide ceramic vapor deposition material, which comprises the steps of preparing silicon source precursor solution and then mixing with SiO 2 And Al 2 O 3 Mixing, ball milling, microwave heat treatment, microwave sintering, compression molding, high-temperature sintering and cooling, wherein the obtained material is not easy to splash during evaporation.
In the prior art, the prepared evaporation material is often uneven in granularity, low in purity and density, and difficult to meet the requirements of the high-end optical coating industry.
Therefore, in order to overcome the defects in the prior art, a preparation method of a silicon oxide evaporation material is needed.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon oxide evaporation material, which can obtain a silicon oxide evaporation material with high purity, high density, uniform granularity and high yield.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a silicon oxide evaporation material, which comprises the following steps:
(1) Mixing silica powder with a binder, and performing ball milling to obtain mixed powder;
(2) Cold isostatic pressing is carried out on the mixed powder obtained in the step (1) to obtain a blank;
(3) Crushing the blank obtained in the step (2) and then sintering to obtain a sintered material;
(4) And (3) classifying and sieving the sintering material obtained in the step (3) to obtain the silicon oxide evaporation material.
The preparation method of the silicon oxide evaporation material adopts a powder metallurgy method, and the silicon oxide evaporation material with high purity, high density, uniform granularity and no slag on the surface can be prepared by molding and sintering the silicon oxide powder, so that the evaporation performance is excellent.
Preferably, the silica powder in step (1) has a purity of 99.99%, such as 99.99%, 99.992%, 99.994%, 99.995%, 99.996%, 99.998% or 99.999%, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the D50 particle size of the silica powder in the step (1) is 1 to 10. Mu.m, for example, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the binder of step (1) comprises sodium silicate and/or polyvinyl alcohol.
Preferably, the binder in step (1) is used in an amount of 0.5 to 6wt% of silica powder, for example, 0.5wt%, 1wt%, 2wt%, 3wt%, 4wt%, 5wt% or 6wt%, but not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
Preferably, the ball-milling material in step (1) has a ball-mass ratio of 1 (3-6), for example, it may be 1:3, 1:3.5, 1:4, 1:4.5, 1:5, 1:5.5 or 1:6, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the rotation speed of the ball milling in the step (1) is 30-80r/min, for example, 30r/min, 40r/min, 50r/min, 60r/min, 70r/min or 80r/min, but the ball milling method is not limited to the listed values, and other non-listed values in the range of values are equally applicable.
Preferably, the ball milling time in the step (1) is equal to or longer than 12h, for example, 12h, 15h, 18h, 20h, 25h, 30h, 40h or 50h, but not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
Preferably, the cold isostatic pressure in step (2) is 180-280MPa, for example 180MPa, 200MPa, 220MPa, 240MPa, 260MPa or 280MPa, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the cold isostatic pressing in step (2) takes 2-8min, for example, 2min, 3min, 4min, 5min, 6min, 7min or 8min, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the end point of the comminution in step (3) is that the particle size of the particles is in the range of 6-10mm, for example 6mm, 7mm, 8mm, 9mm or 10mm, but not limited to the values recited, other values not recited in the range of values being equally applicable.
Preferably, the sintered charge thickness of step (3) is <15mm, which may be, for example, 2mm, 5mm, 8mm, 10mm, 12mm or 14mm, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the sintering of step (3) is performed in an atmosphere of oxygen.
Preferably, the temperature rising rate of the sintering in the step (3) is 1-8 ℃ per minute, for example, 1 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min, 6 ℃/min, 7 ℃/min or 8 ℃/min, but the sintering is not limited to the listed values, and other values not listed in the numerical range are applicable.
Preferably, the sintering in step (3) includes sequentially performing a first sintering, a second sintering, and a third sintering.
Preferably, the temperature of the first sintering is 200-400 ℃, for example, 200 ℃, 250 ℃, 300 ℃, 350 ℃ or 400 ℃, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the time of the first sintering is 0.5-2h, for example, 0.5h, 0.8h, 1h, 1.2h, 1.5h, 1.8h or 2h, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the temperature of the second sintering is 1000-1300 ℃, for example, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, or 1300 ℃, but the second sintering is not limited to the listed values, and other non-listed values in the numerical range are equally applicable.
Preferably, the second sintering time is 0.5-2h, for example, 0.5h, 0.8h, 1h, 1.2h, 1.5h, 1.8h or 2h, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the temperature of the third sintering is 1400-1650 ℃, for example 1400 ℃, 1450 ℃, 1500 ℃, 1550 ℃, 1600 ℃, or 1650 ℃, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the third sintering time is 10-14h, for example, 10h, 11h, 12h, 13h or 14h, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
In the sintering process, through the bonding among powder particles, the free energy of the pore surfaces of the blank is reduced, so that the further densification of the silicon oxide blank is realized.
Preferably, the preparation method further comprises: and dedusting the silicon oxide evaporation material.
The special equipment is used for removing dust from the evaporation material, and floating dust on the surface of the particles is taken away by airflow with a certain pressure.
Preferably, the dust removal time is 10-30min, for example, 10min, 15min, 20min, 25min or 30min, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the silica evaporation material in step (4) has a particle size ranging from 2mm to 5mm, for example, 2mm, 3mm, 4mm or 5mm, but not limited to the recited values, and other values not recited in the range are equally applicable.
As a preferred technical scheme of the preparation method provided by the invention, the preparation method comprises the following steps:
(1) Mixing silica powder with the purity of more than or equal to 99.99 percent and the D50 particle diameter of 1-10 mu m with a binder and water, and then performing ball milling, wherein the dosage of the binder is 0.5-6wt% of the silica powder, the ball milling rotating speed is 30-80r/min, the ball milling time is more than or equal to 12 hours, and the ball material mass ratio during ball milling is 1 (3-6), so as to obtain mixed powder;
(2) Carrying out cold isostatic pressing on the mixed powder obtained in the step (1) for 2-8min under the pressure of 180-280MPa to obtain a blank;
(3) Crushing the blank obtained in the step (2) until the particle size is 6-10mm, and then sintering, wherein the loading thickness is less than 15mm during sintering, the sintering process comprises the steps of firstly heating to 200-400 ℃ at the speed of 5-8 ℃/min under the oxygen atmosphere, preserving heat for 0.5-2h, then heating to 1000-1300 ℃ at the speed of 2-5 ℃/min, preserving heat for 0.5-2h, heating to 1400-1650 ℃ at the speed of 1-3 ℃/min, preserving heat for 10-14h, and cooling along with a furnace to obtain a sintered material;
(4) And (3) classifying and sieving the sintering material obtained in the step (3) and removing dust for 10-30min to obtain the silicon oxide evaporation material with the particle size range of 2-5mm.
Compared with the prior art, the invention has the beneficial effects that:
the silicon oxide evaporation material prepared by the preparation method provided by the invention has high purity and high density, can reach more than 99.0%, has uniform granularity and no slag on the surface, and has stable performance and good evaporation effect when being applied to evaporation.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
In order to clearly illustrate the technical scheme of the invention, the porosity of the silicon oxide evaporation material provided by the embodiment of the invention is detected to determine the density, the uniformity of the particle size distribution of the silicon oxide evaporation material is evaluated by sieving the silicon oxide evaporation material by using a screen with a corresponding mesh, and whether slag exists on the surface of the silicon oxide evaporation material is observed.
Example 1
The embodiment provides a preparation method of a silicon oxide evaporation material, which comprises the following steps:
(1) Selecting high-purity silica powder, wherein the D50 particle size is 5 mu m, the purity is 99.99%, the analytically pure sodium silicate is selected as a binder, the dosage is 3wt% of the silica powder, the binder and 10wt% of pure water of the silica powder are put into a ball mill to be ball-milled at the rotating speed of 50r/min, the ball mass ratio during ball milling is 1:5, the ball milling is carried out for 15 hours, and mixed powder is taken out after the ball milling is finished;
(2) Filling the mixed powder obtained in the step (1) into a rubber sleeve for cold isostatic pressing, wherein the pressure is 250MPa, the dwell time is 5min, and taking out a blank after the cold isostatic pressing is finished;
(3) Placing the blank obtained in the step (2) into a jaw crusher with a ceramic lining for crushing, wherein the particle size is 6-10mm, placing the crushed particles into an alumina crucible, wherein the loading thickness is 12mm when loading, placing the crucible into an oxygen atmosphere sintering furnace, firstly heating to 300 ℃ at the speed of 6 ℃/min, preserving heat for 1h, then heating to 1200 ℃ at the speed of 4 ℃/min, preserving heat for 1h, finally heating to 1500 ℃ at the speed of 2 ℃/min, preserving heat for 12h, and taking out the crucible and the sintering material after cooling to room temperature along with the furnace after the heat preservation is finished;
(4) And (3) classifying and sieving the sintering material obtained in the step (3), and carrying out dust removal for 20min to obtain the silicon oxide evaporation material with the particle size range of 2-5mm.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 2
The embodiment provides a preparation method of a silicon oxide evaporation material, which comprises the following steps:
(1) Selecting high-purity silica powder, wherein the D50 particle size is 10 mu m, the purity is 99.99%, selecting analytically pure polyvinyl alcohol as a binder, using 0.5wt% of the silica powder, putting the silica powder, the binder and 10wt% of pure water of the silica powder into a ball mill, ball milling at a rotating speed of 80r/min, wherein the ball material mass ratio during ball milling is 1:6, ball milling is carried out for 12 hours, and taking out mixed powder after the ball milling is finished;
(2) Filling the mixed powder obtained in the step (1) into a rubber sleeve for cold isostatic pressing, wherein the pressure is 180MPa, the dwell time is 8min, and taking out a blank after the cold isostatic pressing is finished;
(3) Placing the blank obtained in the step (2) into a jaw crusher with a ceramic lining for crushing, wherein the particle size is 6-10mm, placing the crushed particles into an alumina crucible, wherein the loading thickness is 14mm when loading, placing the crucible into an oxygen atmosphere sintering furnace, heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 2h, heating to 1000 ℃ at a speed of 2 ℃/min, preserving heat for 2h, heating to 1400 ℃ at a speed of 1 ℃/min, preserving heat for 14h, cooling to room temperature along with the furnace after the heat preservation is finished, and taking out the crucible and the sintering material;
(4) And (3) classifying and sieving the sintering material obtained in the step (3), and carrying out dust removal for 10min to obtain the silicon oxide evaporation material with the particle size range of 2-5mm.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 3
The embodiment provides a preparation method of a silicon oxide evaporation material, which comprises the following steps:
(1) Selecting high-purity silica powder, wherein the D50 particle size is 1 mu m, the purity is 99.99%, the analytically pure polyvinyl alcohol is selected as a binder, the dosage is 6wt% of the silica powder, the binder and 10wt% of pure water of the silica powder are put into a ball mill to be ball-milled at a rotating speed of 30r/min, the ball mass ratio during ball milling is 1:3, the ball milling is carried out for 20 hours, and mixed powder is taken out after the ball milling is finished;
(2) Filling the mixed powder obtained in the step (1) into a rubber sleeve for cold isostatic pressing, wherein the pressure is 280MPa, the dwell time is 2min, and taking out a blank after the cold isostatic pressing is finished;
(3) Placing the blank obtained in the step (2) into a jaw crusher with a ceramic lining for crushing, wherein the particle size is 6-10mm, placing the crushed particles into an alumina crucible, wherein the loading thickness is 14mm when loading, placing the crucible into an oxygen atmosphere sintering furnace, heating to 400 ℃ at a speed of 8 ℃/min, preserving heat for 0.5h, heating to 1300 ℃ at a speed of 5 ℃/min, preserving heat for 0.5h, heating to 1650 ℃ at a speed of 3 ℃/min, preserving heat for 10h, cooling to room temperature along with the furnace, and taking out the crucible and the sintering material;
(4) And (3) classifying and sieving the sintering material obtained in the step (3), and carrying out dust removal for 30min to obtain the silicon oxide evaporation material with the particle size range of 2-5mm.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 4
This example provides a method for preparing a vaporized material of silicon oxide, which is similar to example 1 except that the pressure of cold isostatic pressing in step (2) is controlled to 150MPa, as compared with example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 5
This example provides a method for preparing a vaporized material of silicon oxide, which is similar to example 1 except that the pressure of cold isostatic pressing in step (2) is controlled to 300MPa, as compared with example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 6
The present example provides a method for preparing a silica vapor, which is similar to example 1 except that the sintering temperature in step (3) is always 1500 ℃ as compared with example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 7
The present example provides a method for preparing a silica vapor material, which is similar to example 1 except that the third sintering temperature in step (3) is 1300 ℃ compared to example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 8
This example provides a method for preparing a silica vapor, which is similar to example 1 except that the third sintering temperature in step (3) is controlled to 1800 ℃.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Example 9
This example provides a method for preparing a silica vapor material, which is comparable to example 1, without dusting, and the remainder is identical to example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Comparative example 1
This comparative example provides a method for preparing a vaporized silicon oxide material without performing the cold isostatic pressing of step (2) in comparison with example 1, and the rest is the same as in example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
Comparative example 2
This comparative example provides a method for producing a silica vapor material, which is similar to example 1 except that the sintering of step (3) is not performed as compared to example 1.
The results of the detection of the silica evaporation material prepared in this example are shown in Table 1.
TABLE 1
| Density (%) | Uniformity of particle size distribution | With or without slag on the surface | |
| Example 1 | 99.5 | Uniformity of | Slag-free |
| Example 2 | 99.0 | Uniformity of | Slag-free |
| Example 3 | 99.7 | Uniformity of | Slag-free |
| Example 4 | 98.2 | Uniformity of | With slag |
| Example 5 | 99.4 | Non-uniformity of | Slag-free |
| Example 6 | 99.5 | Non-uniformity of | Slag-free |
| Example 7 | 97.0 | Non-uniformity of | With slag |
| Example 8 | - | - | - |
| Example 9 | 99.3 | Uniformity of | With slag |
| Comparative example 1 | 81.6 | Non-uniformity of | With slag |
| Comparative example 2 | 58.9 | Not formed into shape | With slag |
In the table "-" indicates no data.
As can be seen from table 1:
the silicon oxide evaporation material provided by the embodiments 1-3 of the invention has good density, the density is more than 99.0%, the granularity distribution is even, the surface is free from slag, the quality of the evaporation material is good, and the evaporation material has good evaporation effect; in example 4, when the pressure of the cold isostatic pressing is too low, it is difficult to achieve the densification effect and the density is lowered as compared with example 1; in example 5, when the pressure of the cold isostatic pressing is too high, the particles are larger and the uniformity is poor; in example 6, sintering was performed at a higher temperature at all times, so that the particles were larger and not uniform; in example 7, when the third sintering temperature is too low, it is difficult to achieve further densification, and both the density and uniformity are lowered; in example 8, when the third sintering temperature is too high, the evaporation material is melted and cannot be used; in example 9, the evaporation material contained excessive slag without dust removal, which reduced the performance; compared with the embodiment 1, the compactness and uniformity of the comparative example 1 and the comparative example 2 are obviously reduced, which indicates that the cold isostatic pressing and sintering process cooperatively improve the performance of the evaporation material, which is indispensable.
In conclusion, the silicon oxide evaporation material prepared by the preparation method provided by the invention has high purity and high density, particularly can reach more than 99.0%, has uniform granularity, has no slag on the surface, and has stable performance and good evaporation effect when being applied to evaporation.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (10)
1. The preparation method of the silicon oxide evaporation material is characterized by comprising the following steps:
(1) Mixing silica powder with a binder, and performing ball milling to obtain mixed powder;
(2) Cold isostatic pressing is carried out on the mixed powder obtained in the step (1) to obtain a blank;
(3) Crushing the blank obtained in the step (2) and then sintering to obtain a sintered material;
(4) And (3) classifying and sieving the sintering material obtained in the step (3) to obtain the silicon oxide evaporation material.
2. The method according to claim 1, wherein the silica powder in step (1) has a purity of 99.99% or more;
preferably, the D50 particle size of the silica powder in the step (1) is 1-10 mu m.
3. The method of claim 1 or 2, wherein the binder of step (1) comprises sodium silicate and/or polyvinyl alcohol;
preferably, the binder in step (1) is used in an amount of 0.5 to 6wt% of silica powder.
4. The preparation method according to any one of claims 1 to 3, wherein the ball mill in the step (1) has a ball mass ratio of 1 (3 to 6);
preferably, the rotating speed of the ball milling in the step (1) is 30-80r/min;
preferably, the ball milling time in the step (1) is more than or equal to 12 hours.
5. The method according to any one of claims 1 to 4, wherein the cold isostatic pressure in step (2) is 180-280MPa;
preferably, the cold isostatic pressing of step (2) takes 2-8min.
6. The method of any one of claims 1-5, wherein the end point of the comminution in step (3) is that the particle size of the particles is in the range of 6-10mm;
preferably, the sintered charge thickness of step (3) is <15 mm;
preferably, the sintering of step (3) is performed in an atmosphere of oxygen.
7. The method according to any one of claims 1 to 6, wherein the temperature rise rate of the sintering in step (3) is 1 to 8 ℃/min;
preferably, the sintering in step (3) includes a first sintering, a second sintering and a third sintering which are sequentially performed;
preferably, the temperature of the first sintering is 200-400 ℃;
preferably, the time of the first sintering is 0.5-2h;
preferably, the temperature of the second sintering is 1000-1300 ℃;
preferably, the second sintering time is 0.5-2h;
preferably, the temperature of the third sintering is 1400-1650 ℃;
preferably, the time of the third sintering is 10-14h.
8. The method of any one of claims 1-7, wherein the method further comprises: dedusting the silicon oxide evaporation material;
preferably, the dust removal time is 10-30min.
9. The method according to any one of claims 1 to 8, wherein the silica evaporation material in step (4) has a particle diameter ranging from 2 to 5mm.
10. The preparation method according to any one of claims 1 to 9, characterized in that the preparation method comprises the steps of:
(1) Mixing silica powder with the purity of more than or equal to 99.99 percent and the D50 particle diameter of 1-10 mu m with a binder and water, and then performing ball milling, wherein the dosage of the binder is 0.5-6wt% of the silica powder, the ball milling rotating speed is 30-80r/min, the ball milling time is more than or equal to 12 hours, and the ball material mass ratio during ball milling is 1 (3-6), so as to obtain mixed powder;
(2) Carrying out cold isostatic pressing on the mixed powder obtained in the step (1) for 2-8min under the pressure of 180-280MPa to obtain a blank;
(3) Crushing the blank obtained in the step (2) until the particle size is 6-10mm, and then sintering, wherein the thickness of the material to be charged is less than 15mm, and the sintering process comprises the steps of firstly heating to 200-400 ℃ at the speed of 5-8 ℃/min under the oxygen atmosphere, preserving heat for 0.5-2h, then heating to 1000-1300 ℃ at the speed of 2-5 ℃/min, preserving heat for 0.5-2h, heating to 1400-1650 ℃ at the speed of 1-3 ℃/min, preserving heat for 10-14h, and cooling along with a furnace to obtain a sintered material;
(4) And (3) classifying and sieving the sintering material obtained in the step (3) and removing dust for 10-30min to obtain the silicon oxide evaporation material with the particle size range of 2-5mm.
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| CN114768971A (en) * | 2022-03-29 | 2022-07-22 | 宁波江丰电子材料股份有限公司 | Germanium evaporation material and preparation method and application thereof |
| CN115124330A (en) * | 2022-07-04 | 2022-09-30 | 宁波江丰电子材料股份有限公司 | Preparation method of silicon oxide ceramic target blank |
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| CN112811908A (en) * | 2021-03-17 | 2021-05-18 | 上海戎创铠迅特种材料有限公司 | Silicon carbide composite target material and preparation method thereof |
| CN114768971A (en) * | 2022-03-29 | 2022-07-22 | 宁波江丰电子材料股份有限公司 | Germanium evaporation material and preparation method and application thereof |
| CN115124330A (en) * | 2022-07-04 | 2022-09-30 | 宁波江丰电子材料股份有限公司 | Preparation method of silicon oxide ceramic target blank |
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