CN106835024B - A method of preparing non-evaporable film getter - Google Patents
A method of preparing non-evaporable film getter Download PDFInfo
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- CN106835024B CN106835024B CN201710009732.0A CN201710009732A CN106835024B CN 106835024 B CN106835024 B CN 106835024B CN 201710009732 A CN201710009732 A CN 201710009732A CN 106835024 B CN106835024 B CN 106835024B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0214—Compounds of V, Nb, Ta
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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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
- C23C14/06—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
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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
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
- C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
- C23C14/546—Controlling the film thickness or evaporation rate using measurement on deposited material using crystal oscillators
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Abstract
Present invention discloses a kind of methods for preparing non-evaporable film getter, several getter metals one-to-one correspondence is placed in several evaporation boats of coating machine as target, getter metals are at least two kinds, the running parameter of each evaporation boat is individually controllable, it is corresponded at each evaporation boat and is equipped with film thickness monitor, to monitor the evaporation rate of getter metals in corresponding evaporation boat；Substrate and evaporation boat are put into the vacuum chamber of coating machine；To being vacuumized in vacuum chamber；Fritting is carried out to getter metals, and the running parameter for controlling each evaporation boat makes each getter metals while evaporating；The evaporation rate of each getter metals is adjusted to default ratio by the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor.The present invention can evaporate a variety of getter metals simultaneously, without additional production alloy, be beneficial to save preparation cost and the time of getter, meanwhile, by controlling the evaporation rate of each getter metals, it can accurately control the ingredient of getter.
Description
Technical field
The present invention relates to a kind of preparation methods of film getter, and in particular to a kind of to prepare non-evaporable film getter
Method.
Background technique
Getter, also referred to as getter, certain gases point can effectively be absorbed using the physically or chemically characteristic of itself by referring to
The common name of the preparation or device of son, for obtaining, maintaining vacuum and purified gases.Getter is widely used in needing vacuum environment
Photoelectric device in, create good working environment for device, stabilize the characteristic parameters of device, performance to device and make
There is important influence with the service life.
Getter is generally divided into evaporable and non-evaporable two major classes, wherein evaporable air-absorbing agent mainly passes through chemical anti-
Residual activity gas in vacuum device should be absorbed, needs to heat getter metals, evapotranspiring out forms getter film；Non-evaporable
Getter does not need getter metals to evapotranspire out, but by making it have gettering ability to getter metals surface activation.Often
Material as nonevaporable getter is mainly by the getter metals structure such as titanium, zirconium, hafnium, vanadium, aluminium, transition metal, rare earth element
At two-spot or multicomponent alloy.
Currently, the main preparation methods of non-evaporable film getter are as follows: each getter metals, melting is in proportion first
Alloy, or each getter metals are pressed into alloy and are annealed again, then by alloy deposition by way of sputtering or evaporating
Film-type getter is prepared in substrate surface.These methods add additional workload and cost, in addition when making alloy
Need to control its uniformity and granularity.
Also have preparation method be a variety of getter metals filament windings together, sputtered, due to the physics of each getter metals
Characteristic is different, and evolution ratio is different when sputtering or evaporating, and final getter has obvious difference at branch and theoretical value.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing non-evaporable film getter.
For achieving the above object, the present invention adopts the following technical scheme:
A method of preparing non-evaporable film getter, comprising the following steps:
S1, several getter metals one-to-one correspondence is placed in several evaporation boats of coating machine as target, getter metals
At least two kinds, the running parameter of each evaporation boat is individually controllable, corresponds at each evaporation boat and is equipped with film thickness monitor, with monitoring
The evaporation rate of getter metals in corresponding evaporation boat；
S2, substrate and evaporation boat are put into the vacuum chamber of coating machine；
S3, to being vacuumized in vacuum chamber；
S4, fritting is carried out to getter metals, and the running parameter for controlling each evaporation boat makes each getter metals while evaporating；
S5, the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor, by the evaporation speed of each getter metals
Rate is adjusted to default ratio.
Technical solution as a further improvement of that present invention, the film thickness monitor are crystal oscillator.
Technical solution as a further improvement of that present invention, getter metals described in step S1 be titanium, zirconium, vanadium, tantalum, niobium,
Iron, aluminium, copper, in molybdenum it is any two or more.
Technical solution as a further improvement of that present invention, getter metals are three kinds in step S1, are titanium, zirconium, vanadium respectively,
The quantity of evaporation boat and film thickness monitor is all three；
Titanium in step S5, zirconium, vanadium evaporation rate ratio be 3.874:3.845:2.281.
Technical solution as a further improvement of that present invention, it is zirconium, vanadium and iron respectively that getter metals, which are three kinds, in step S1,
The quantity of evaporation boat and film thickness monitor is all three；
The evaporation rate ratio of zirconium, vanadium and iron is 6.960:2.608:0.432 in step S5.
Technical solution as a further improvement of that present invention, getter metals are two kinds in step S1, are zirconium, aluminium respectively, steam
The quantity for sending out boat and film thickness monitor is all two；
Zirconium in step S5, aluminium evaporation rate ratio be 6.784:3.216.
Compared with the existing technology, the technical effects of the invention are that:
The present invention can evaporate a variety of getter metals simultaneously, without additional production alloy, be beneficial to save the system of getter
Standby cost and time, meanwhile, by controlling the evaporation rate of each getter metals, it can accurately control the ingredient of getter.
Specific embodiment
Below with reference to specific embodiment, the present invention will be described in detail.But these embodiments are not intended to limit this hair
Bright, structure that those skilled in the art are made according to these embodiments, method or transformation functionally include
Within the scope of the present invention.
One embodiment of the present invention presented below:
A method of preparing non-evaporable film getter, comprising the following steps:
S1, several getter metals one-to-one correspondence is placed in several evaporation boats of coating machine as target, getter metals
At least two kinds, the running parameter of each evaporation boat is individually controllable, corresponds at each evaporation boat and is equipped with film thickness monitor, with monitoring
The evaporation rate of getter metals in corresponding evaporation boat；
S2, substrate and evaporation boat are put into the vacuum chamber of coating machine；
S3, to being vacuumized in vacuum chamber；
S4, fritting is carried out to getter metals, and the running parameter for controlling each evaporation boat makes each getter metals while evaporating；
S5, the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor, by the evaporation speed of each getter metals
Rate is adjusted to default ratio.
The working time of evaporation boat is the overall thickness of controllable film getter in rate-determining steps S5.
It should be noted that the running parameter of evaporation boat is the power of evaporation boat.
When carrying out fritting to getter metals, joined by evaporating temperature, quality, specific heat capacity of getter metals in each evaporation boat etc.
Number can calculate to obtain power of each evaporation boat when carrying out fritting, so that each getter metals evaporate simultaneously.
Film thickness monitor real-time monitoring corresponds to the evaporation rate of getter metals in evaporation boat, rate ratio and default ratio phase
Corresponding evaporation boat power is increased when relatively low, then reduces corresponding evaporation boat power when rate ratio is higher compared with default ratio.
Default ratio is obtained according to ingredient (atomic percentage) Extrapolation of getter metals each in getter finished product,
It is specific as follows, atomic percentage is corresponding be each getter metals in getter finished product content, pass through containing for each getter metals
Amount can calculate the quality of each getter metals, and the volume of each getter metals can be calculated further according to the density of each getter metals, because
Identical (being equal to chip area) in the area of deposition on substrate for each getter metals, then the percent by volume of each getter metals is equal to
Percentage thickness, the percentage thickness are the default ratio for being proportional to evaporation rate.
Further, the film thickness monitor is crystal oscillator.
Further, getter metals described in step S1 be titanium, zirconium, vanadium, tantalum, niobium, iron, aluminium, copper, in molybdenum any two kinds or
It is two or more.
The present invention can evaporate a variety of getter metals simultaneously, without additional production alloy, be beneficial to save the system of getter
Standby cost and time, meanwhile, by controlling the evaporation rate of each getter metals, it can accurately control the ingredient of getter.
Embodiment 1
It is titanium, zirconium, vanadium that the present embodiment, which is used to prepare getter metals, and the atomic fraction percentage of titanium, zirconium, vanadium is 40%:
The getter of 30%:30%, according to can be calculated titanium, zirconium, vanadium percentage thickness be 38.74%:38.45%:22.81%,
Then titanium, zirconium, vanadium evaporation rate preset ratio be 3.874:3.845:2.281.
A method of preparing non-evaporable film getter, comprising the following steps:
S1, three kinds of titanium, zirconium, vanadium getter metals one-to-one correspondence are placed in three evaporation boats of coating machine as target,
The running parameter of each evaporation boat is individually controllable, corresponds at each evaporation boat and is equipped with film thickness monitor, to monitor corresponding evaporation boat
The evaporation rate of interior getter metals；
S2, substrate and evaporation boat are put into the vacuum chamber of coating machine；
S3, to being vacuumized in vacuum chamber；
S4, drop to 10 to vacuum degree-3Fritting is carried out to getter metals after Pa, and the running parameter for controlling each evaporation boat makes
Each getter metals evaporate simultaneously；
S5, the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor, by the evaporation rate of titanium, zirconium, vanadium
It is adjusted to 3.874:3.845:2.281.
Embodiment 2
It is zirconium, vanadium and iron that the present embodiment, which is used to prepare getter metals, and the atomic fraction percentage of zirconium, vanadium and iron is 57%:
The getter of 36%:7% is 69.60%:26.08%:4.32% according to the percentage thickness that can be calculated zirconium, vanadium and iron, then
It is 6.960:2.608:0.432 that the evaporation rate of zirconium, vanadium and iron, which presets ratio,.
A method of preparing non-evaporable film getter, comprising the following steps:
S1, three kinds of getter metals one-to-one correspondence of zirconium, vanadium and iron are placed in three evaporation boats of coating machine as target,
The running parameter of each evaporation boat is individually controllable, corresponds at each evaporation boat and is equipped with film thickness monitor, to monitor corresponding evaporation boat
The evaporation rate of interior getter metals；
S2, substrate and evaporation boat are put into the vacuum chamber of coating machine；
S3, to being vacuumized in vacuum chamber；
S4, drop to 10 to vacuum degree-3Fritting is carried out to getter metals after Pa, and the running parameter for controlling each evaporation boat makes
Each getter metals evaporate simultaneously；
S5, the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor, by the evaporation rate of zirconium, vanadium and iron
It is adjusted to 6.960:2.608:0.432.
Embodiment 3
It is zirconium, aluminium that the present embodiment, which is used to prepare getter metals, and the atomic fraction percentage of zirconium, aluminium is 60%:40%'s
Getter is 67.84%:32.16% according to the percentage thickness that can be calculated zirconium, aluminium, then the default ratio of evaporation rate of zirconium, aluminium
Value is 6.784:3.216.
A method of preparing non-evaporable film getter, comprising the following steps:
S1, two kinds of zirconium, aluminium getter metals one-to-one correspondence are placed in two evaporation boats of coating machine as target, it is each to steam
The running parameter for sending out boat is individually controllable, corresponds at each evaporation boat and is equipped with film thickness monitor, to monitor corresponding evaporation boat interior suction
The evaporation rate of gas metal；
S2, substrate and evaporation boat are put into the vacuum chamber of coating machine；
S3, to being vacuumized in vacuum chamber；
S4, drop to 10 to vacuum degree-3Fritting is carried out to getter metals after Pa, and the running parameter for controlling each evaporation boat makes
Each getter metals evaporate simultaneously；
S5, the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor, the evaporation rate of zirconium, aluminium is adjusted
For 6.784:3.216.
Finally, it should be noted that embodiment of above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
Invention is explained in detail referring to aforementioned embodiments for pipe, those skilled in the art should understand that: its according to
It can so modify to technical solution documented by aforementioned each embodiment, or part of technical characteristic is equal
Replacement；And these are modified or replaceed, each embodiment technical solution of the present invention that it does not separate the essence of the corresponding technical solution
Spirit and scope.
Claims (1)
1. a kind of method for preparing non-evaporable film getter, which comprises the following steps:
S1, several getter metals one-to-one correspondence is placed in several evaporation boats of coating machine as target, the getter metals
It is three kinds, is titanium, zirconium, vanadium respectively, the quantity of evaporation boat is three, and the running parameter of each evaporation boat is individually controllable, each evaporation boat
Place, which corresponds, is equipped with film thickness monitor, to monitor the evaporation rate of getter metals in corresponding evaporation boat；
S2, substrate and evaporation boat are put into the vacuum chamber of coating machine；
S3, to being vacuumized in vacuum chamber；
S4, fritting is carried out to getter metals, and the running parameter for controlling each evaporation boat makes each getter metals while evaporating；
S5, the running parameter that evaporation boat is adjusted according to the value of feedback of film thickness monitor, by the evaporation rate of titanium, zirconium, vanadium than adjusting
Whole is 3.874: 3.845: 2.281；
The film thickness monitor is crystal oscillator.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111621671B (en) * | 2020-06-18 | 2022-03-15 | 南京哲玺太电子科技有限公司 | Zirconium series non-evaporable getter and preparation method and application thereof |
| CN112342501B (en) * | 2020-09-15 | 2022-01-04 | 中国科学院高能物理研究所 | Preparation method of Pd/Ti double-layer getter film and Pd/Ti double-layer getter film |
| CN112144030A (en) * | 2020-09-16 | 2020-12-29 | 上海晶维材料科技有限公司 | Titanium-based rare earth alloy target and preparation method thereof |
| CN113699425B (en) * | 2021-08-31 | 2022-07-15 | 中国科学技术大学 | Non-evaporable quaternary Ti-Zr-V-Cu vacuum getter film and preparation method thereof |
| CN114011374B (en) * | 2021-11-03 | 2023-07-14 | 安徽有研吸气材料有限公司 | Fast-suction non-evaporable titanium-molybdenum getter |
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|---|---|---|---|---|
| CN103849835A (en) * | 2012-11-29 | 2014-06-11 | 北京有色金属研究总院 | Zr-Co-Re thin film getter provided with protection layer, and preparation method thereof |
| CN103898463A (en) * | 2014-03-07 | 2014-07-02 | 浙江大学 | Multi-element high-entropy alloy film and preparation method thereof |
| CN104532190A (en) * | 2014-12-19 | 2015-04-22 | 合肥工业大学 | Preparation method of Zr-Cu metal glass film |
| CN105177468A (en) * | 2015-08-24 | 2015-12-23 | 合肥工业大学 | Cu-Ag amorphous alloy film and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6016159B2 (en) * | 2012-12-21 | 2016-10-26 | 大学共同利用機関法人 高エネルギー加速器研究機構 | Non-evaporable getter pump |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849835A (en) * | 2012-11-29 | 2014-06-11 | 北京有色金属研究总院 | Zr-Co-Re thin film getter provided with protection layer, and preparation method thereof |
| CN103898463A (en) * | 2014-03-07 | 2014-07-02 | 浙江大学 | Multi-element high-entropy alloy film and preparation method thereof |
| CN104532190A (en) * | 2014-12-19 | 2015-04-22 | 合肥工业大学 | Preparation method of Zr-Cu metal glass film |
| CN105177468A (en) * | 2015-08-24 | 2015-12-23 | 合肥工业大学 | Cu-Ag amorphous alloy film and preparation method thereof |
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Address after: 2-1-b, 2-2-b, phase III, Zhongxin Technology Industrial Park, no.6, Louyang Road, Suzhou Industrial Park, Jiangsu Province Patentee after: Suzhou Houpu Sensing Technology Co.,Ltd. Address before: 2-1-b, 2-2-b, phase III, Zhongxin Technology Industrial Park, no.6, Louyang Road, Suzhou Industrial Park, Jiangsu Province Patentee before: SUZHOU JINGXING PHOTOELECTRIC TECHNOLOGY CO.,LTD. |