EP3112315B1 - Method for filling csac absorption cells with high-purity alkali metal - Google Patents
Method for filling csac absorption cells with high-purity alkali metal Download PDFInfo
- Publication number
- EP3112315B1 EP3112315B1 EP14884030.9A EP14884030A EP3112315B1 EP 3112315 B1 EP3112315 B1 EP 3112315B1 EP 14884030 A EP14884030 A EP 14884030A EP 3112315 B1 EP3112315 B1 EP 3112315B1
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- EP
- European Patent Office
- Prior art keywords
- alkali metal
- silicon wafer
- glass
- absorption
- cavities
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052783 alkali metal Inorganic materials 0.000 title claims description 68
- 150000001340 alkali metals Chemical class 0.000 title claims description 67
- 238000010521 absorption reaction Methods 0.000 title claims description 52
- 238000000034 method Methods 0.000 title claims description 30
- 229910052710 silicon Inorganic materials 0.000 claims description 33
- 239000010703 silicon Substances 0.000 claims description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
- 150000001339 alkali metal compounds Chemical class 0.000 claims description 23
- 239000005357 flat glass Substances 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052792 caesium Inorganic materials 0.000 claims description 4
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 229910052701 rubidium Inorganic materials 0.000 claims description 4
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 3
- 238000005452 bending Methods 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 description 34
- 239000000758 substrate Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000001427 coherent effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- -1 silicon alkali metal Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000005472 transition radiation Effects 0.000 description 2
- 241001247287 Pentalinon luteum Species 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G04—HOROLOGY
- G04F—TIME-INTERVAL MEASURING
- G04F5/00—Apparatus for producing preselected time intervals for use as timing standards
- G04F5/14—Apparatus for producing preselected time intervals for use as timing standards using atomic clocks
Definitions
- the present invention relates to a method for filling wafer-based chip-scale atomic clock absorption cells with a high-purity alkali metal.
- Time measurement relates to two quantities-epochs and time intervals. Any natural phenomena with periodical changes can be used to measure time.
- timing instruments have also constantly developed with humans' progress over 3,500 years, people's demand for timing accuracy is becoming higher and higher.
- people developed sundials which take advantage of the periodic change law of earth rotation to identify time changes, then sand clocks, astronomical clock towers, mechanical pendulum clocks, quartz clocks, atomic clocks and optical clocks. It is clear that all of them use the natural phenomena with periodic changes to measure time.
- An atomic clock is an instrument which realizes accurate time measurement by using atomic transition radiation frequency between hyperfine energy levels in the atomic ground state.
- the miniature atomic clock based on the CPT (Coherent Population Trapping) phenomenon is an inexorable development trend of atomic clock miniaturization. And the miniaturization of its core chip alkalis metal vapor cavity plays a critical role in the miniaturization of the atomic clock.
- the technical methods for filling micro absorption cells with an alkali metal can mainly be divided into two categories.
- One category is to directly inject a pure alkali metal (such as rubidium and cesium) into the absorption cell.
- This category needs an sophisticated large vacuum equipment and a strict vacuum environment. A trace of residual oxygen in the cavity may lead to the oxidization of the alkali metal and then reduce the service life of the atomic clocks.
- the second category is to directly inject alkali metal compounds into the absorption cell cavity to produce the corresponding alkali metal through chemical reactions.
- This category needs to strictly control the amount of the compounds which are injected into the absorption cell while the residual impurities of the reactions may remain in the absorption cell and then affect the atomic clock performance.
- the two categories share the same disadvantage: absorption cells need to be filled one by one so it is difficult to realize production on a large scale.
- the present invention puts forward a method for filling wafer-based chip-scale atomic clock absorption cells with a high-purity alkali metal.
- the present invention aims at overcoming the problem of the prior art that alkali metals are extremely prone to oxidization during the production of atomic clock absorption cells.
- An atomic clock is an instrument which realizes accurate time measurement by using atomic transition radiation frequency between hyperfine energy levels in the atomic ground state.
- the miniature atomic clock based on the CPT (Coherent Population Trapping) phenomenon is an inexorable development trend of atomic clock miniaturization. And the miniaturization of its core chip alkalis metal vapor cavity plays a critical role in the miniaturization of the atomic clock.
- JP 2013 125907 A discloses a method of manufacturing a gas cell of an atomic oscillator.
- the gas cell consists of a first substrate made of glass, a second substrate made of silicon, and a third substrate.
- the method includes: forming a connecting groove, a first through hole, and a second through hole on the silicon substrate, wherein the first through hole and the second through hole penetrate the silicon substrate, and are connected to each other through the connecting groove; bonding the first substrate to one surface of the second substrate, placing an alkali metal generating agent in the second through hole, and bonding the third substrate to the other surface of the second substrate; irradiating the alkali metal generating agent by using a laser light to generate alkali metal gas, and filling the first through hole with the alkali metal gas; deforming the first substrate in the region where the connecting groove is formed and to eliminate the space between the first through hole and the second through hole, and enclosing the alkali metal gas in the first through hole.
- US 2012/243088 A1 recites a gas cell manufacturing method.
- the method includes: arranging solid substances at a plurality of holes each of which is provided on each of a plurality of cells; accommodating gas in inner spaces of the cells through an air flow path connected to the holes; and sealing the spaces by melting the solid substances to close the holes.
- US 7 893 780 B2 discloses an alkali beam cell system including a reversible alkali beam cell.
- the reversible alkali beam cell includes: a first chamber configured as a reservoir chamber to evaporate an alkali metal during a first time period and as a detection chamber to collect the evaporated alkali metal during a second time period; a second chamber configured as the detection chamber during the first time period and as the reservoir chamber during the second time period; and an aperture interconnecting the first and the second chambers.
- the technical methods for filling micro absorption cells with an alkali metal can mainly be divided into two categories.
- One category is to directly inject a pure alkali metal (such as rubidium and cesium) into the absorption cell.
- This category needs a sophisticated large vacuum equipment and a strict vacuum environment. A trace of residual oxygen in the cavity may lead to the oxidization of the alkali metal and then reduce the service life of the atomic clocks.
- the second category is to directly inject alkali metal compounds into the absorption cell cavity to produce the corresponding alkali metal through chemical reactions.
- This category needs to strictly control the amount of the compounds which are injected into the absorption cell while the residual impurities of the reactions may remain in the absorption cell and then affect the atomic clock performance.
- the two categories share the same disadvantage: absorption cells need to be filled one by one so it is difficult to realize production on a large scale.
- the present invention puts forward a method for filling wafer-based chip-scale atomic clock absorption cells with a high-purity alkali metal.
- the present invention aims at overcoming the problem of the prior art that alkali metals are extremely prone to oxidization during the production of atomic clock absorption cells.
- the present invention realizes the filling of all absorption cells on the wafer at the same time to meet the demand for large-scale production of atomic clocks.
- the present invention is characterized by low cost and high efficiency.
- the present invention defines a method according to claim 1.
- a preferred embodiment of the present invention is defined in claim 2.
- the invention has the advantages of easy processes and rapid, low-cost, large-scale production of atomic clock alkali metal absorption cells.
- 101 double-side polished silicon wafers; 102. shallow micro grooves; 103. alkali metal compound placement cavities; 104. alkali metal absorption cell cavities; 105. sheet glass A; 106. alkali metal compounds; 107. sheet glass B; 108. temporary micro flow channels; 109. alkali metal vapor; 110. equipment for partial cooling; 111. high-purity solid alkali metal; 201. high-purity alkali metal; 202. silicon alkali metal absorption cell cavities; 203. upper-layer glass; and 204. lower-layer glass.
- the glass-silicon-glass three-layer wafer level anodic bonding technique which is used in the present invention is carried out in two steps: the first step is to form temporary micro flow channels for alkali metal vapor; and the second step is to reuse the anodic bonding technique to realize the sealing of the alkali metal compound.
- make the alkali metal compound in the placement cavities react chemically by separately adjusting the temperature of the placement cavities to produce high-purity alkali metal through decomposition.
- the intensity of decomposition reactions can be controlled by adjusting the temperature of the alkali metal placement cavities.
- the flow channel of the alkali metal vapor is that the alkali metal vapor diffuses into the absorption cell through silicon-glass temporary micro flow channel and congeals in the absorption cell through partial cooling.
- a shallow micro groove 102 which is 1-2 ⁇ m in depth and 80-90 mm in diameter on one side of a 4-cun double-side polished silicon wafer 101, and an alkali metal compound placement cavity 103 which is 20 mm in diameter at the center of the double-side polished silicon wafer 101.
- the alkali metal compound placement cavity 103 and the alkali metal absorption cell cavity 104 both have a through-hole structure, running through the double-side polished silicon wafer 101, as shown in FIG. 1a .
- the alkali metal vapor 109 diffuses in the whole cavity including the alkali metal absorption cell cavity 104 through the temporary micro flow channel 108.
- An equipment for partial cooling 110 can adjust the temperature of the double-side polished silicon wafer 101 excluding the alkali metal compound placement cavity 103.
- the alkali metal vapor 109 congeals at the bottom of the alkali metal absorption cell cavity 104 to become a high-purity solid alkali metal 111 used to fill the alkali metal absorption cell cavity 104, as shown in FIG. 1c .
- the atomic clock alkali metal absorption cells made by the wafer level technique can be cut into individual atomic clock alkali metal absorption cells by slicing the wafer.
- a high-purity alkali metal 201 is placed in a silicon alkali metal absorption cell cavity 202 which is sealed by an upper-layer glass 203 and a lower glass 204.
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Micromachines (AREA)
- Engineering & Computer Science (AREA)
- Stabilization Of Oscillater, Synchronisation, Frequency Synthesizers (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Piezo-Electric Or Mechanical Vibrators, Or Delay Or Filter Circuits (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410067976.0A CN103864007B (zh) | 2014-02-27 | 2014-02-27 | 在片实现芯片级原子钟吸收泡的高纯度碱金属填充方法 |
PCT/CN2014/000816 WO2015127577A1 (zh) | 2014-02-27 | 2014-09-02 | 在片实现芯片级原子钟吸收泡的高纯度碱金属填充方法 |
Publications (4)
Publication Number | Publication Date |
---|---|
EP3112315A1 EP3112315A1 (en) | 2017-01-04 |
EP3112315A4 EP3112315A4 (en) | 2017-03-08 |
EP3112315A8 EP3112315A8 (en) | 2017-06-28 |
EP3112315B1 true EP3112315B1 (en) | 2021-07-14 |
Family
ID=50903111
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14884030.9A Active EP3112315B1 (en) | 2014-02-27 | 2014-09-02 | Method for filling csac absorption cells with high-purity alkali metal |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP3112315B1 (zh) |
KR (1) | KR101824789B1 (zh) |
CN (1) | CN103864007B (zh) |
WO (1) | WO2015127577A1 (zh) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103864007B (zh) | 2014-02-27 | 2016-03-30 | 中国电子科技集团公司第五十五研究所 | 在片实现芯片级原子钟吸收泡的高纯度碱金属填充方法 |
CN104609364B (zh) * | 2015-01-28 | 2016-05-11 | 中国科学院上海光学精密机械研究所 | 高精度混合缓冲气体碱金属原子蒸汽泡的制作方法及系统 |
CN107840305B (zh) * | 2017-11-13 | 2019-05-10 | 北京无线电计量测试研究所 | 一种芯片原子钟的mems原子腔的制作方法 |
CN111855579B (zh) * | 2019-04-28 | 2024-06-11 | 核工业理化工程研究院 | 一种碱金属原子蒸气吸收池及其光谱测量方法 |
CN114477074A (zh) * | 2021-12-22 | 2022-05-13 | 北京自动化控制设备研究所 | 基于mems技术的晶圆级原子气室加工方法及装置 |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050007118A1 (en) * | 2003-04-09 | 2005-01-13 | John Kitching | Micromachined alkali-atom vapor cells and method of fabrication |
US7666485B2 (en) * | 2005-06-06 | 2010-02-23 | Cornell University | Alkali metal-wax micropackets for alkali metal handling |
DE102007034963B4 (de) * | 2007-07-26 | 2011-09-22 | Universität des Saarlandes | Zelle mit einer Kavität und einer die Kavität umgebenden Wandung, Verfahren zur Herstellung einer derartigen Zelle, deren Verwendung und Wandung mit einer darin ausbildbaren Ausnehmung |
US7893780B2 (en) * | 2008-06-17 | 2011-02-22 | Northrop Grumman Guidance And Electronic Company, Inc. | Reversible alkali beam cell |
US8258884B2 (en) * | 2009-12-22 | 2012-09-04 | Teledyne Scientific & Imaging, Llc | System for charging a vapor cell |
US8299860B2 (en) * | 2010-02-04 | 2012-10-30 | Honeywell International Inc. | Fabrication techniques to enhance pressure uniformity in anodically bonded vapor cells |
JP5699725B2 (ja) * | 2011-03-23 | 2015-04-15 | セイコーエプソン株式会社 | ガスセル製造装置およびガスセルの製造方法 |
CN102259825B (zh) * | 2011-06-17 | 2015-04-08 | 清华大学 | 一种mems原子蒸气腔室的制备方法及原子蒸气腔室 |
JP6031787B2 (ja) * | 2011-07-13 | 2016-11-24 | 株式会社リコー | 原子発振器の製造方法 |
CN102323738B (zh) * | 2011-07-20 | 2014-04-02 | 中国科学院上海微系统与信息技术研究所 | 一种采用mems工艺制作的槽型原子气体腔及其构造的原子钟物理系统 |
JP5961998B2 (ja) * | 2011-12-15 | 2016-08-03 | 株式会社リコー | 原子発振器の製造方法 |
CN102515084A (zh) * | 2011-12-30 | 2012-06-27 | 东南大学 | 微流控原子腔、片上原子钟芯片及制备方法 |
CN102515083A (zh) * | 2011-12-30 | 2012-06-27 | 东南大学 | 有光入射平面的微型原子腔、微型原子钟芯片及制备方法 |
CN102491259A (zh) * | 2011-12-30 | 2012-06-13 | 东南大学 | Mems微型原子腔、微型原子钟芯片及制备方法 |
CN103342335B (zh) * | 2013-06-21 | 2015-10-07 | 中国科学院上海微系统与信息技术研究所 | 一种微型cpt原子钟碱金属蒸汽腔的充气和封堵系统及方法 |
CN103864007B (zh) | 2014-02-27 | 2016-03-30 | 中国电子科技集团公司第五十五研究所 | 在片实现芯片级原子钟吸收泡的高纯度碱金属填充方法 |
-
2014
- 2014-02-27 CN CN201410067976.0A patent/CN103864007B/zh active Active
- 2014-09-02 EP EP14884030.9A patent/EP3112315B1/en active Active
- 2014-09-02 KR KR1020157036179A patent/KR101824789B1/ko active IP Right Grant
- 2014-09-02 WO PCT/CN2014/000816 patent/WO2015127577A1/zh active Application Filing
Non-Patent Citations (1)
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Also Published As
Publication number | Publication date |
---|---|
CN103864007A (zh) | 2014-06-18 |
KR20160013122A (ko) | 2016-02-03 |
CN103864007B (zh) | 2016-03-30 |
EP3112315A8 (en) | 2017-06-28 |
EP3112315A1 (en) | 2017-01-04 |
KR101824789B1 (ko) | 2018-02-01 |
WO2015127577A1 (zh) | 2015-09-03 |
EP3112315A4 (en) | 2017-03-08 |
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