CN109988996B - Preparation method of P-type ZnO film - Google Patents
Preparation method of P-type ZnO film Download PDFInfo
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- CN109988996B CN109988996B CN201810003796.4A CN201810003796A CN109988996B CN 109988996 B CN109988996 B CN 109988996B CN 201810003796 A CN201810003796 A CN 201810003796A CN 109988996 B CN109988996 B CN 109988996B
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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
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
Abstract
The invention relates to the field of preparation of P-type ZnO films,in the prior art, the P-type ZnO film is not easy to prepare; the invention provides a preparation method of a P-type ZnO film, which comprises the following steps: mixing Mg3N2ZnO and ZnO are respectively arranged on the target material substrate in the reaction chamber, and a first reaction area and a second reaction area are respectively formed between the ZnO and the target material substrate by separating the ZnO and the ZnO; a substrate with a clean surface is placed on the substrate base plate; the substrate base plate can rotate and carries the substrate to periodically circulate between the two reaction areas when rotating; and B: determining reaction conditions of the reaction chamber; step C, rotating the substrate base plate to make the substrate periodically circulate for 250-350 times between the two reaction areas; alternately sputtering and growing a ZnO film on the surface of the substrate during the circulation period, wherein the thickness of the finally obtained P-type ZnO film is between 300 and 350 nm; in the step C, in a cycle period of the substrate, the time of the substrate in the first reaction zone is 0.1-6s, and the time of the substrate in the second reaction zone is 25-35 s; the P-type ZnO film can be easily prepared.
Description
Technical Field
The invention relates to the field of preparation of P-type ZnO films, in particular to a preparation method of a P-type ZnO film.
Background
The LED light emission gradually develops from visible red light to blue light, and white light emission is realized through the cooperation of fluorescent powder. The shorter the wavelength is, the stronger the luminous energy is, and the luminous energy is applied to illumination and display screens, so that the luminous intensity and the definition can be greatly improved. ZnO has a forbidden bandwidth of 3.37eV, and is expected to further shorten the wavelength of the LED and realize ultraviolet light emission.
For this purpose, P-type and N-type ZnO films are required to be prepared as chips to realize ultraviolet light emission. The N-type ZnO thin film can be formed by doping a pentavalent element such as Al or Ga. However, since ZnO tends to have oxygen vacancies during the growth process, it is difficult to obtain a P-type ZnO thin film. In order to obtain P-type ZnO thin films, trivalent elements in 5 groups are generally doped, wherein N and O have close sizes and are the most promising elements for realizing P-type ZnO thin films in the 5 groups. However, in practice, the hole density of ZnO to N is low, and it is difficult to prepare a P-type ZnO film.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a preparation method of a P-type ZnO film, so that the P-type ZnO film can be obtained easily.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a P-type ZnO film comprises the following steps: separating the reaction chamber of the magnetic control reaction device by a baffle plate to form two reaction zones which are respectively a first reaction zone and a second reaction zoneA reaction zone and a second reaction zone; placing Mg on the target material substrate of the first reaction zone3N2As a target material, ZnO is placed on the target material substrate of the second reaction area as the target material; disposing a substrate within said reaction chamber alternately movable between said first reaction zone and said second reaction zone; and B: the vacuum degree of the reaction chamber is pumped to 1.3X 10-4Pa; with N2And O2Is a sputtering atmosphere, N2And O2The flow ratio of (2) is 100: 2, maintaining the air pressure of the reaction chamber at 2.6 +/-0.1 Pa; the temperature of a substrate base plate is 100 +/-2 ℃; the radio frequency power of the first reaction zone is 20-100W, and the radio frequency power of the second reaction zone is 25-35W; step C, the substrate is alternately circulated between the two reaction areas for 250-350 times; alternately sputtering and growing a ZnO film on the surface of the substrate during the circulation period, wherein the thickness of the finally obtained P-type ZnO film is between 300 and 350 nm; in the step C, in one cycle period of the substrate, the time of the substrate in the first reaction zone is 0.1-6s, and the time of the substrate in the second reaction zone is 25-35 s.
By adopting the technical scheme, the two reaction areas are separated by the baffle, when the two reaction areas are subjected to magnetron sputtering simultaneously, the substrate only receives sputtering particles of the target material in the current reaction area due to the existence of the baffle, and the sputtering particles of the target material in the other reaction area are blocked by the baffle in the process of flying to the substrate; the substrate is periodically and circularly rotated to respectively circulate between the two reaction areas, and the surface of the substrate alternately sputters to grow a P-type ZnO film.
The further preferable scheme of the invention is as follows: the reaction chamber is internally provided with a substrate base plate which is opposite to and parallel to the target base plate, the substrate is fixed on the surface of the substrate base plate, and the substrate base plate can rotate and can drive the substrate to alternately move between the two reaction areas when rotating.
Through being fixed in the surface of rotatable substrate base plate with the substrate, only need just can drive the rotation of substrate base plate and come control cycle through the rotational speed of motor through a motor, simple structure, easy operation.
The further preferable scheme of the invention is as follows: in the step C, the radio frequency power of the first reaction zone is 30-90W; the substrate is in the first reaction zone for 0.2-5s during one cycle of the substrate.
The further preferable scheme of the invention is as follows: in the step C, the radio frequency power of the first reaction zone is 50W.
The further preferable scheme of the invention is as follows: in the step C, the radio frequency power of the first reaction zone is 70W.
The further preferable scheme of the invention is as follows: the doping proportion of Mg in the obtained ZnO film is 5-14%.
The further preferable scheme of the invention is as follows: the doping proportion of Mg in the obtained ZnO film is 20-33%.
The further preferable scheme of the invention is as follows: in the step C, the radio frequency power of the second reaction zone is 30W.
The further preferable scheme of the invention is as follows: in the step C, the radio frequency time of the second reaction zone is 30 s.
The further preferable scheme of the invention is as follows: the cycle number in the step C is 300; in the first cycle, the substrate begins to be located in the second reaction zone.
In conclusion, the invention has the following beneficial effects: and the substrate rotates to ensure that the ZnO film is alternately sputtered and grown on the surface of the substrate when the substrate circularly shuttles between the first reaction area and the second reaction area. When the substrate is positioned in the second reaction zone, ZnO crystal lattices are sputtered and grown on the surface of the substrate; as the substrate rotates into the first reaction zone, sputtered particles (containing Mg) come into contact with the ZnO lattice and are displaced.
Drawings
FIG. 1 is a schematic diagram of the preparation of a P-type ZnO film;
FIG. 2 is Mg at 0.2S3N2A plot of sputtering power as a function of film resistivity;
FIG. 3 shows different sputtering powers (Mg) at 0.2S3N2) As a function of the c-axis lattice size;
FIGS. 4 and 5 are Mg at sputtering powers of 50W and 70W, respectively3N2A plot of the deposition period;
FIG. 6 is a graph plotting the forbidden band widths of films obtained under 4 conditions.
In the figure: 1. a magnetic control reaction device; 2. a target substrate; 3. a substrate base plate; 4. a substrate; 5. and a baffle plate.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications without inventive contribution to the present embodiment as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
As shown in fig. 1, a magnetron reaction apparatus 1 for preparing a P-type ZnO film is shown, a reaction chamber of the magnetron reaction apparatus 1 is cylindrical, a substrate 3 is disposed on an upper bottom surface of the reaction chamber, two target substrates 2 are disposed on lower bottom surfaces of the reaction chamber, and the substrate 3 and the two target substrates 2 are disposed in parallel and opposite to each other. A baffle 5 is vertically arranged between the two target material substrates 2 to divide the reaction chamber into two reaction areas, wherein the two reaction areas are a first reaction area and a second reaction area respectively; placing Mg on the target substrate 2 of the first reaction zone3N2As a target material, ZnO is placed on the target material substrate 2 of the second reaction area as a target material; a substrate 4 with a clean surface is arranged on the substrate base plate 3, the upper bottom surface of the substrate 4 is fixed with the substrate base plate 3, and the lower bottom surface of the substrate 4 faces the target base plate 2 below; the substrate base plate 3 can rotate around the center of the reaction chamber and alternately (cyclically) move between the two reaction zones with the substrate 4 while rotating. The substrate base plate 3 may be replaced with a rotatable arm having one end of a circular shape with respect to the center of the reaction chamber and the other end rotatable (or swingably reciprocated) about the center of the reaction chamber in the horizontal direction, and the substrate 4 is fixed to one end of the arm and alternately moved between the two reaction chambers during the movement to the arm.
A preparation method of a P-type ZnO film uses the device and comprises the following steps,
step A: separating a reaction chamber of a magnetic control reaction device by using a baffle plate to form two reaction zones, wherein the two reaction zones are a first reaction zone and a second reaction zone respectively; placing Mg on the target material substrate of the first reaction zone3N2As a target material, in the second reactionZnO is placed on the target material substrate of the area as a target material; disposing a substrate within said reaction chamber alternately movable between said first reaction zone and said second reaction zone;
and B: the vacuum degree of the reaction chamber is pumped to 1.3X 10-4Pa; with N2And O2Is a sputtering atmosphere, N2And O2The flow ratio of (2) is 100: 2, maintaining the air pressure of the reaction chamber at 2.6 +/-0.1 Pa; the temperature of the substrate base plate 3 is 100 +/-2 ℃; the radio frequency power of the first reaction zone is 20-100W, and the radio frequency power of the second reaction zone is 25-35W;
step C, rotating the substrate base plate to make the substrate alternately circulate between the two reaction areas for 250-350 times; alternately sputtering and growing a ZnO film on the surface of the substrate during the circulation period, wherein the thickness of the finally obtained P-type ZnO film is between 300 and 350 nm;
in step C, the time that the substrate is positioned in the first reaction zone in one cycle period of the substrate is 0.1-6s (namely, single cycle Mg3N2Deposition period) of 25-35s (deposition period of single cycle ZnO).
The specific working principle is as follows: by rotating the substrate base plate 3, the ZnO film is alternatively sputtered and grown on the surface of the substrate 4 when the substrate is circularly shuttled between the first reaction area and the second reaction area. When the substrate is positioned in the second reaction zone, ZnO crystal lattices are sputtered and grown on the surface of the substrate; when the substrate 4 rotates to the first reaction zone, sputtering particles (containing Mg) contact with ZnO crystal lattices and are substituted, and the doping condition of Mg in the P-type thin film is controlled by controlling the sputtering power of the first reaction zone and the sputtering time of the substrate 4 in the first reaction zone. The doping proportion of Mg in the P-type film is respectively in positive correlation with the sputtering power of the first reaction area and the sputtering receiving time of the substrate 4 in the first reaction area, and the forbidden bandwidth of the ZnO film is in positive correlation with the doping proportion of Mg. Therefore, the ZnO film which meets the forbidden bandwidth can be obtained by selecting the proper Mg doping proportion range.
According to the preparation method of the P-type ZnO film, the following experiments are respectively carried out:
firstly, determining the sputtering power of a second reaction area to be 30W; in one cycle period of the substrate, the time for which the substrate is positioned in the first reaction zone is 0.2s, and the time for which the substrate is positioned in the second reaction zone is 30 s; selecting 30W, 50W, 60W,70W and 90W as the sputtering power of the first reaction area in sequence, respectively carrying out experiments 1 to 5 under the condition that other experimental conditions are not changed, wherein the experimental results are as follows,
(1) growth rate
Mg3N2: mg on a substrate at 100 DEG C3N2The growth rate of the film and the thickness contributed in each cycle were calculated. Since the growth atmosphere contains oxygen, the obtained thin film is MgNxOy in fact. (e.g., RF =50W, x =0.5, y = 0.25; RF =30W, x =0.1, y = 0.85) Mg on a substrate3N2The growth rates at different sputtering powers are shown in the following table:
ZnO, deposition rate (nm/s) 0.033 nm/s; the thickness contributed in each cycle was 1 nm.
(2) Sputtering (RF) power (Mg)3N2) Dependence on film properties and resistivity (see FIG. 2 for details)
The sputtering power of the first reaction zone is 50-70W, the number of the Seebeck coefficient is measured to be 0.5-0.4mV/K,
it was confirmed that a P-type thin film was obtained. The resistivity of the film at this time was 9.9X 103-4.5×103Ωcm。
(3) Results of XRD (grid size, see FIG. 3 for details)
Results by XRD for different sputtering powers (Mg)3N2) The c-axis lattice size of the film was calculated.
Defect-free ZnO film, c-axis lattice size is 5.207A.
As the sputtering power was increased to 30W and 50W, the size of the lattice became large because of the decrease in oxygen vacancies.
The sputtering power is increased to 60W,70W and 90W, the grid size is gradually reduced, and Mg is doped into ZnO (the doping of N has little influence on the size)
Secondly, determining the sputtering power of the second reaction area to be 30W; in one cycle period of the substrate, the time that the substrate is positioned in the second reaction zone is 30s, and the time that the substrate is positioned in the first reaction zone is 2s and 5s respectively; sequentially selecting 50W and 70W as the sputtering power of the first reaction area, respectively carrying out experiments 6 to 9 under the condition that other experimental conditions are not changed,
(4) exploring Mg3N2The effect of growth time (sputtering power 50W and 70W) and the experimental results are as follows (detailed description)
See figures 4 and 5),
Mg3N2the growth time of (2) was added with two conditions of 2s and 5 s.
The film was at 0.2s, 2s and 5s Mg with a sputtering power of 50W3N2The p-type characteristic is shown under the growth time. Lowest resistivity of 4.5X 103Omega cm occurs at growth time 2 s.
At a sputtering power of 70W, the film is only 0.2s of Mg3N2The p-type characteristic is shown under the growth time.
Accompanied by Mg3N2The growth time increased, and the lattice size decreased for both 50W and 70W. The largest reduction in lattice size occurred at 70W,5s because of the substitution of Mg for ZnO in the lattice.
(5) Forbidden band width
The films obtained under the four conditions were subjected to (alpha hv)2And (4) plotting a photon energy relation graph, and obtaining the forbidden band width of each film (see figure 6 in detail).
The forbidden band width is 3.31eV under the conditions of 50W and 0.2 s; the forbidden band width is 3.37eV under the conditions of 50W and 5 s. The forbidden band width increases with increasing growth time.
This tendency is more pronounced at a sputtering power of 70W. The forbidden band widths of 0.2s and 5s are 3.48eV and 3.59eV, respectively.
The numerical calculation of the forbidden band width can be known to be 50W; in the case of 0.2s and 5s, the doping ratios of Mg in the obtained p-type thin film were 5% and 14%. At 70W; in the case of 0.2s and 5s, the doping ratio of Mg was 20% and 33%.
Claims (10)
1. A preparation method of a P-type ZnO film is characterized by comprising the following steps,
step A: separating a reaction chamber of a magnetic control reaction device by using a baffle plate to form two reaction zones, wherein the two reaction zones are a first reaction zone and a second reaction zone respectively; placing Mg on the target material substrate of the first reaction zone3N2As a target material, ZnO is placed on the target material substrate of the second reaction area as the target material; disposing a substrate within said reaction chamber alternately movable between said first reaction zone and said second reaction zone;
and B: the vacuum degree of the reaction chamber is pumped to 1.3X 10-4Pa; with N2And O2Is a sputtering atmosphere, N2And O2The flow ratio of (2) is 100: 2, maintaining the air pressure of the reaction chamber at 2.6 +/-0.1 Pa; the temperature of a substrate base plate is 100 +/-2 ℃; the radio frequency power of the first reaction zone is 20-100W, and the radio frequency power of the second reaction zone is 25-35W;
step C, the substrate is alternately circulated between the two reaction areas for 250-350 times; alternately sputtering and growing a ZnO film on the surface of the substrate during the circulation period, wherein the thickness of the finally obtained P-type ZnO film is between 300 and 350 nm;
in the step C, in one cycle period of the substrate, the time of the substrate in the first reaction zone is 0.1-6s, and the time of the substrate in the second reaction zone is 25-35 s.
2. The method for producing a thin film according to claim 1, wherein: the reaction chamber is internally provided with a substrate base plate which is opposite to and parallel to the target base plate, the substrate is fixed on the surface of the substrate base plate, and the substrate base plate can rotate and can drive the substrate to alternately move between the two reaction areas when rotating.
3. The method for producing a thin film according to claim 2, wherein: in the step C, the radio frequency power of the first reaction zone is 30-90W; the substrate is in the first reaction zone for 0.2-5s during one cycle of the substrate.
4. The method for producing a thin film according to claim 3, wherein: in the step C, the radio frequency power of the first reaction zone is 50W.
5. The method for producing a thin film according to claim 3, wherein: in the step C, the radio frequency power of the first reaction zone is 70W.
6. The method for producing a thin film according to claim 4, wherein: the doping proportion of Mg in the obtained ZnO film is 5-14%.
7. The method for producing a thin film according to claim 5, wherein: the doping proportion of Mg in the obtained ZnO film is 20-33%.
8. The method for producing a thin film according to any one of claims 2 to 7, wherein: in the step C, the radio frequency power of the second reaction zone is 30W.
9. The method for producing a thin film according to claim 8, wherein: in the step C, the radio frequency time of the second reaction zone is 30 s.
10. The method for producing a thin film according to claim 9, wherein: the cycle number in the step C is 300; in the first cycle, the substrate begins to be located in the second reaction zone.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101135044A (en) * | 2006-12-11 | 2008-03-05 | 中国科学院上海硅酸盐研究所 | Method for preparing stable cavity type zinc oxide film by jigger coupling sputtering |
| CN101768728A (en) * | 2010-01-15 | 2010-07-07 | 深圳大学 | Method for preparing doped ZnO-based film through magnetron sputtering |
| JP2012059874A (en) * | 2010-09-08 | 2012-03-22 | Stanley Electric Co Ltd | MANUFACTURING METHOD OF ZnO-BASED SEMICONDUCTOR LAYER AND MANUFACTURING METHOD OF ZnO-BASED SEMICONDUCTOR LIGHT-EMITTING ELEMENT |
| CN103160785A (en) * | 2013-03-01 | 2013-06-19 | 溧阳华晶电子材料有限公司 | Manufacture method for nitrogen-magnesium co-doping p-type zinc oxide film |
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- 2018-01-03 CN CN201810003796.4A patent/CN109988996B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135044A (en) * | 2006-12-11 | 2008-03-05 | 中国科学院上海硅酸盐研究所 | Method for preparing stable cavity type zinc oxide film by jigger coupling sputtering |
| CN101768728A (en) * | 2010-01-15 | 2010-07-07 | 深圳大学 | Method for preparing doped ZnO-based film through magnetron sputtering |
| JP2012059874A (en) * | 2010-09-08 | 2012-03-22 | Stanley Electric Co Ltd | MANUFACTURING METHOD OF ZnO-BASED SEMICONDUCTOR LAYER AND MANUFACTURING METHOD OF ZnO-BASED SEMICONDUCTOR LIGHT-EMITTING ELEMENT |
| CN103160785A (en) * | 2013-03-01 | 2013-06-19 | 溧阳华晶电子材料有限公司 | Manufacture method for nitrogen-magnesium co-doping p-type zinc oxide film |
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