CN101210313A - Method for growing MgxZn1-xO film by electron-beam evaporation - Google Patents
Method for growing MgxZn1-xO film by electron-beam evaporation Download PDFInfo
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- CN101210313A CN101210313A CNA2006101733895A CN200610173389A CN101210313A CN 101210313 A CN101210313 A CN 101210313A CN A2006101733895 A CNA2006101733895 A CN A2006101733895A CN 200610173389 A CN200610173389 A CN 200610173389A CN 101210313 A CN101210313 A CN 101210313A
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Abstract
The invention belongs to the field of semiconductor photoelectric material technology and relates to a method for growing an MgxZn1-xO film by electron beam evaporation. A composite target formed by sintering polycrystalline MgO and ZnO powder is evaporated by electron beam heating by electron beam evaporating equipment and is deposed on a substrate to form the MgxZn1-xO semiconductor alloy thin film. The invention has simple preparation process and low cost, and is suitable for preparing thin film used for UV detectors with wavelength of 280 to 220 nm.
Description
Technical field:
The invention belongs to the photoelectric semiconductor material technical field, relate to a kind of employing electron beam evaporation (electron beam evaporation) equipment growth Mg
xZn
1-xA kind of method of O semiconductor alloy film.
Background technology:
Along with reaching its maturity of infrared countermeasure technique, rate is subjected to serious threat in the accuracy at target of infrared guidance and the standard of infrared warning, therefore, and deep ultraviolet wave band (day blind area in recent years, 280-220nm) the detector development begins in succession in world developed country, and makes substantial progress.Because the solar radiation in this wave band district (280-220nm) in our atmospheric layer, especially is zero substantially,, form so-called " day blind area " so this wave band is not subjected to influenced by solar in the near-earth atmosphere surface.So the signal that under a kind of like this background, detects, it is highly sensitive, good reliability.
Mg
xZn
1-xThe O film is novel semiconductor material with wide forbidden band, it is a kind of broad-band gap ternary semiconductor material, when taking into account ZnO, MgO material property, have the continuously adjustable characteristics of band gap, be particularly suitable for the needs of the ultraviolet light solid ultraviolet detector of detecting band between 280-220nm.Compare Mg with III-V group-III nitride wide-band gap material
xZn
1-xGrowth substrates, growth temperature that O sosoloid has coupling are low, and radiation resistance is stronger, and abundant raw material, and cost is low, and is pollution-free, inherent advantages such as Heat stability is good.Its energy gap is adjustable continuously from 3.3～7.8eV in addition.
Mg
xZn
1-xThe O ternary alloy is formed by certain component solid solution by ZnO and MgO.ZnO is a wurtzite structure, hexagonal system, lattice parameter a=0.325nm, c=0.521nm; MgO is the NaCl structure, isometric system, lattice parameter a=0.424nm.Because Zn
2+(0.060nm) and Mg
2+(0.057nm) ionic radius is approaching, Mg
2+And Zn
2+In each autoxidisable substance lattice, replace mutually and form Mg
xZn
1-xThe lattice distortion that O instead type mixed crystal causes is less.With Mg content difference, Mg
xZn
1-xO can be partial to a certain crystalline network, and Mg content＜37% is hex crystal structure (lattice parameter and ZnO is approaching, and a slightly increases, and c slightly reduces), and＞62% is cubic crystal structure (lattice parameter and MgO are close, and a slightly reduces), is mixed phase between the two.Mg content greater than 37% less than 62% high quality Mg
xZn
1-xThe O film has the major application meaning on ultraviolet detection, but Mg content is at this interval Mg
xZn
1-xThe O film preparation is difficulty very.At present, preparation Mg
xZn
1-xThe O film mainly contains pulsed laser deposition (PLD), magnetron sputtering, molecular beam epitaxy (MBE), metal organic chemical vapor deposition methods such as (MOCVD), and the equipment great majority that these methods are used cost an arm and a leg complicated operation.
Summary of the invention
For the equipment great majority that solve the prior art use cost an arm and a leg, the problem of complicated operation the invention provides a kind of electron beam evaporation growth Mg
xZn
1-xThe method of O film utilizes electron beam evaporation equipment to make composition target that sintering polycrystalline MgO and ZnO powder form through electron beam heating evaporation, is deposited on the substrate, forms Mg
xZn
1-xO semiconductor alloy film, preparation technology is simple, and cost is low.
The present invention is characterised in that and comprises the following steps:
(a) be 5%～50% ratio mixing with ZnO and MgO powder in the molar content of MgO, make round pie, burn till the MgZnO ceramic block at 1000 ℃～1300 ℃ with tabletting machine;
(b) the MgZnO ceramic block is put in the crucible of electron beam evaporation equipment, substrate be placed on the MgZnO ceramic block directly over the distance of 8cm～15cm, press on the substrate to add electrothermal stove;
(c) shut bell jar, vacuumize with coating equipment, substrate is heated to a certain temperature between room temperature～500 ℃; When coating equipment vacuum tightness reaches 3 * 10
-3During Pa, begin growth;
(d) open each switch on the electrical control cubicles in order, regulate electron beam and make it focus on the spot minimum of MgZnO ceramic block; Adjusting heater current, high pressure make the line value at 20mA～40mA, and air pressure remains on 2 * 10
-2Pa--3 * 10
-2Pa;
(e) remove plate washer and pick up counting, the time reaches 10 minutes～after 1 hour, closes each switch on the electrical control cubicles in proper order by shutdown, takes out deposition Mg
xZn
1-xThe substrate of O semiconductor alloy film.
Beneficial effect: the present invention utilizes electron beam evaporation equipment to make composition target that sintering polycrystalline MgO and ZnO powder form through electron beam heating evaporation, is deposited on the substrate, forms Mg
xZn
1-xO semiconductor alloy film, preparation technology is simple, and cost is low; Electron beam source and substrate separately can avoid sputtering method to cause the sputter damage of film in the sputter, are suitable for preparing the film that ultraviolet detector is used that is suitable for of 280nm-220nm wave band.
Embodiment
The invention will be further described below by embodiment:
Embodiment 1, and under different growth temperatures, Mg grows on quartz substrate
xZn
1-xThe O film:
At first be with acetone, ethanol, deionized water quartz substrate to be carried out supersound washing to handle, and use high-purity N
2Dry up, be put on the clamping plate and clip, put into the bell jar crucible directly over the position of 15cm, press the heating electric stove wire above; The MgZnO ceramic block is put in the crucible, puts suitably.Build bell jar, suction reaches 3 * 10
-3Pa begins growth.----------suitably raise and press, strengthen heater current--adjusting deflection X-axis, Y-axis, focusing make the beam spot minimum that shines on the target--strengthens voltage, heater current to 12A preheating filament 5 minutes to filament switch to open high pressure to drive deflection, focusing switch to open the electrical control cubicles power switch; Adjusting heater current, high pressure make line keep 25mA, and vacuum tightness is 2 * 10 in the process of growth
-2Pa is respectively at 290 ℃ of underlayer temperatures, 310 ℃, 350 ℃ or 380 ℃ of growth Mg
xZn
1-xThe O film, growth time 10 minutes.
The film of making is done to absorb and the transmission test, the film of 290 ℃ and 310 ℃ has a very steep ABSORPTION EDGE in the test result between 220nm-240nm, show that film has good quality in the 220nm-240nm wavelength band, also show deposited by electron beam evaporation growth Mg
xZn
1-xThe O film is Mg under different underlayer temperature conditions
xZn
1-xO film band gap difference.
Embodiment 2, change line, and under different evaporation energy, Mg grows on quartz substrate
xZn
1-xThe O film:
With acetone, ethanol, deionized water quartz substrate is carried out supersound washing and handle, and use high-purity N
2Dry up, be put on the clamping plate and clip, put into the bell jar crucible directly over the position of 15cm, press the heating electric stove wire above; The MgZnO ceramic block is put in the crucible, puts suitably.Build bell jar then, suction reaches 3 * 10
-3Pa begins growth.290 ℃ of selection growth temperatures--300 ℃, vacuum tightness is 2 * 10 in the process of growth
-2Pa; Adjusting heater current, high pressure change line, and the line value is respectively 20mA, 30mA or 40mA, makes film growth under different evaporation energy, and growth time is 50 minutes.Because the fusing point of ZnO and MgO is different,, so just can reach the purpose of the ratio of MgO and ZnO in the adjusting film so change the effect that line can reach the vaporator rate of the ZnO that regulates in the MgZnO ceramic block and MgO.To be respectively the Mg that grows under 20mA, 30mA and the 40mA condition in the line value
xZn
1-xThe O film is done and is absorbed test, and the line value is the Mg that grows under the 30mA condition
xZn
1-xThe absorption and the transmission plot of O film are better, ABSORPTION EDGE 234nm, and steep; And the line value is the Mg that grows under 20mA and the 40mA condition
xZn
1-xThe O film is then about 220nm; Show and select suitable line can improve Mg
xZn
1-xThe O film quality also can be regulated Mg
xZn
1-xThe absorption spectrum ranges of O film.
Embodiment 3, MgO in the change MgZnO ceramic block and the mol ratio of ZnO, and Mg grows on quartz
xZn
1-xThe O film:
Because the vapour pressure of MgO and ZnO is different, so the Mg of electron beam growth
xZn
1-xMg content is higher than the Mg content in the MgZnO ceramic block in the O film.290 ℃ of underlayer temperatures--300 ℃, line 30mA, vacuum tightness are 3 * 10
-2The molar content of Pa and MgO is respectively the Mg that grows under 5%, 10%, 20%, 40% or 50% condition
xZn
1-xO film, growth time are 30 minutes.The Mg that grows under the molar content condition to different Mg O
xZn
1-xThe O film is tested, and relative better with 40% outcome quality that obtains with 50% ceramic block, ABSORPTION EDGE is the relative red shift of other component relatively.
Above embodiment substrate can also be selected sapphire.
Be appreciated that to the change of the foregoing description and revise for those skilled in the art be clear and expect among, therefore, should regard top detailed description as example rather than restriction.
Claims (5)
1. electron beam evaporation growth Mg
xZn
1-xThe method of O film is characterized in that comprising the following steps:
(a) ZnO and MgO powder are 5%～50% ratio mixing in the molar content of MgO, make round pie with tabletting machine, burn till the MgZnO ceramic block at 1000 ℃～1300 ℃;
(b) the MgZnO ceramic block is put in the crucible of electron beam evaporation equipment, substrate be placed on the MgZnO ceramic block directly over the distance of 8cm～15cm, press on the substrate to add electrothermal stove;
(c) shut bell jar, vacuumize with coating equipment, substrate is heated to a certain temperature between room temperature～500 ℃;
(d) open each switch on the electrical control cubicles in order, regulate electron beam and make it focus on the spot minimum of MgZnO ceramic block; Adjusting heater current, high pressure make the line value at 20mA～40mA, and air pressure remains on 2 * 10
-2Pa--3 * 10
-2Pa;
(e) remove plate washer and pick up counting, the time reaches 10 minutes～after 1 hour, turns off each switch on the electrical control cubicles by the order of shutdown.
2. electron beam evaporation growth Mg according to claim 1
xZn
1-xThe method of O film is characterized in that vacuum tightness is 2 * 10 in the process of growth
-2Pa or 3 * 10
-2Pa.
3. electron beam evaporation growth Mg according to claim 1
xZn
1-xThe method of O film is characterized in that underlayer temperature is 290 ℃, 310 ℃, 350 ℃ or 380 ℃.
4. electron beam evaporation growth Mg according to claim 1
xZn
1-xThe method of O film is characterized in that the line value is 20mA, 30mA or 40mA.
5. electron beam evaporation growth Mg according to claim 1
xZn
1-xThe method of O film is characterized in that the molar content of MgO in the MgZnO ceramic block is respectively 5%, 10%, 20%, 40% or 50%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101733895A CN101210313A (en) | 2006-12-29 | 2006-12-29 | Method for growing MgxZn1-xO film by electron-beam evaporation |
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|---|---|---|---|
| CNA2006101733895A CN101210313A (en) | 2006-12-29 | 2006-12-29 | Method for growing MgxZn1-xO film by electron-beam evaporation |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101969023A (en) * | 2010-08-04 | 2011-02-09 | 长春理工大学 | Method for making step growth MgxZn1-xO thin film on silicon substrate |
| CN102443765A (en) * | 2010-10-15 | 2012-05-09 | 海洋王照明科技股份有限公司 | Preparation method of MgZnO semiconductor film |
| CN102560362A (en) * | 2012-03-08 | 2012-07-11 | 杭州电子科技大学 | Method for preparing p-type CuAlO2 transparent conductive film |
| CN102586741A (en) * | 2012-03-01 | 2012-07-18 | 大连理工大学 | Preparation method of doped zinc oxide film |
| WO2015050630A2 (en) | 2013-09-18 | 2015-04-09 | Solar-Tectic Llc | Methods of producing large grain or single crystal films |
| US9806125B2 (en) | 2015-07-28 | 2017-10-31 | Carrier Corporation | Compositionally graded photodetectors |
| US9865766B2 (en) | 2015-07-28 | 2018-01-09 | Carrier Corporation | Ultraviolet photodetectors and methods of making ultraviolet photodetectors |
| US9928727B2 (en) | 2015-07-28 | 2018-03-27 | Carrier Corporation | Flame detectors |
| US10126165B2 (en) | 2015-07-28 | 2018-11-13 | Carrier Corporation | Radiation sensors |
| CN109133910A (en) * | 2018-09-13 | 2019-01-04 | 先导薄膜材料（广东）有限公司 | The production method of ZMO target |
| CN116254509A (en) * | 2021-12-10 | 2023-06-13 | 长春理工大学 | Preparation of MgZnO film by electron beam evaporation method |
-
2006
- 2006-12-29 CN CNA2006101733895A patent/CN101210313A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101969023A (en) * | 2010-08-04 | 2011-02-09 | 长春理工大学 | Method for making step growth MgxZn1-xO thin film on silicon substrate |
| CN101969023B (en) * | 2010-08-04 | 2012-05-02 | 长春理工大学 | Method for making step growth MgxZn1-xO thin film on silicon substrate |
| CN102443765A (en) * | 2010-10-15 | 2012-05-09 | 海洋王照明科技股份有限公司 | Preparation method of MgZnO semiconductor film |
| CN102443765B (en) * | 2010-10-15 | 2013-08-07 | 海洋王照明科技股份有限公司 | Preparation method of MgZnO semiconductor film |
| CN102586741A (en) * | 2012-03-01 | 2012-07-18 | 大连理工大学 | Preparation method of doped zinc oxide film |
| CN102586741B (en) * | 2012-03-01 | 2014-04-09 | 大连理工大学 | Preparation method of doped zinc oxide film |
| CN102560362A (en) * | 2012-03-08 | 2012-07-11 | 杭州电子科技大学 | Method for preparing p-type CuAlO2 transparent conductive film |
| EP3047054A4 (en) * | 2013-09-18 | 2017-05-17 | Solar-Tectic, LLC | Methods of producing large grain or single crystal films |
| WO2015050630A2 (en) | 2013-09-18 | 2015-04-09 | Solar-Tectic Llc | Methods of producing large grain or single crystal films |
| US9806125B2 (en) | 2015-07-28 | 2017-10-31 | Carrier Corporation | Compositionally graded photodetectors |
| US9865766B2 (en) | 2015-07-28 | 2018-01-09 | Carrier Corporation | Ultraviolet photodetectors and methods of making ultraviolet photodetectors |
| US9928727B2 (en) | 2015-07-28 | 2018-03-27 | Carrier Corporation | Flame detectors |
| US10126165B2 (en) | 2015-07-28 | 2018-11-13 | Carrier Corporation | Radiation sensors |
| US10718662B2 (en) | 2015-07-28 | 2020-07-21 | Carrier Corporation | Radiation sensors |
| US11029202B2 (en) | 2015-07-28 | 2021-06-08 | Carrier Corporation | Radiation sensors |
| CN109133910A (en) * | 2018-09-13 | 2019-01-04 | 先导薄膜材料（广东）有限公司 | The production method of ZMO target |
| CN109133910B (en) * | 2018-09-13 | 2021-07-20 | 先导薄膜材料（广东）有限公司 | Production method of ZMO target material |
| CN116254509A (en) * | 2021-12-10 | 2023-06-13 | 长春理工大学 | Preparation of MgZnO film by electron beam evaporation method |
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Open date: 20080702 |