CN108695136A - The production method of oxide semiconductor thin-film and application - Google Patents
The production method of oxide semiconductor thin-film and application Download PDFInfo
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- CN108695136A CN108695136A CN201710218074.6A CN201710218074A CN108695136A CN 108695136 A CN108695136 A CN 108695136A CN 201710218074 A CN201710218074 A CN 201710218074A CN 108695136 A CN108695136 A CN 108695136A
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- 239000010409 thin film Substances 0.000 title claims abstract description 123
- 239000004065 semiconductor Substances 0.000 title claims abstract description 109
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 47
- 239000000758 substrate Substances 0.000 claims abstract description 41
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 6
- 230000010148 water-pollination Effects 0.000 claims abstract description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 29
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 29
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 23
- 239000010408 film Substances 0.000 claims description 17
- 229910002651 NO3 Inorganic materials 0.000 claims description 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 4
- 208000011580 syndromic disease Diseases 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- 230000008569 process Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000001259 photo etching Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 23
- 238000010586 diagram Methods 0.000 description 11
- 238000007639 printing Methods 0.000 description 11
- 238000012546 transfer Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000010606 normalization Methods 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 6
- 238000007641 inkjet printing Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- DTSBBUTWIOVIBV-UHFFFAOYSA-N molybdenum niobium Chemical compound [Nb].[Mo] DTSBBUTWIOVIBV-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000003852 thin film production method Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02554—Oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02623—Liquid deposition
- H01L21/02628—Liquid deposition using solutions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Thin Film Transistor (AREA)
Abstract
The invention discloses a kind of production methods of oxide semiconductor thin-film, including:Hydrophobic treatment is carried out to substrate, obtains modified substrate;Prepare electric ink:Functional reagent is added into the precursor solution of oxide semiconductor, obtains electric ink;The functional reagent has both hydrophily and improves viscosity effect;Electric ink is printed on to the surface of modified substrate, forms ink droplet;After ink droplet drying, ink droplet is made annealing treatment, oxide semiconductor thin-film is obtained on modified substrate.The oxide semiconductor thin-film that the production method can form small size, lack thickness;Meanwhile avoiding using vacuum equipment and photoetching process, effectively reduce cost of manufacture.Production method based on the oxide semiconductor thin-film, the present invention also provides a kind of oxide thin film transistors and preparation method thereof, above-mentioned oxide semiconductor thin-film is used as active layer, more oxide thin film transistors can be maximumlly integrated on unit area, meet the high pixel demand of display backboard.
Description
Technical field
The invention belongs to electronic material and device arts, in particular, being related to a kind of oxide semiconductor thin-film
The application of production method and the oxide semiconductor thin-film in oxide thin film transistor.
Background technology
Oxide thin film transistor has become the display of a new generation due to the advantage that its stability is good, preparation temperature is low
Backboard actuation techniques.In oxide thin film transistor, key structure, that is, oxide semiconductor thin-film.High performance oxide half
Vacuum deposition preparation not only may be used in conductor thin film, ink jet printing can also be used to prepare;Wherein, it is prepared using printing technology
The oxide semiconductor thin-film is avoided using vacuum equipment and photoetching process, is had many advantages, such as simple for process and of low cost.
If wanting to realize the display panel that LCD and OLED can be driven luminous, need to integrate a large amount of TFT devices in unit area,
This proposes very high requirement to the size of single TFT devices and duty ratio etc..For example, 55 cun of 4K display screens require single picture
The size of vegetarian refreshments is about 300 μm of 100 μ m, this is made that prodigious limitation to the size of thin film transistor (TFT).As in TFT devices
Most important structure, active layer array needs to control size less than 50 μm, and oxide TFT prepared by solwution method is to wherein active
The thickness of layer, which needs to control, is less than 30nm.Usually using the ink-jet printing apparatus that inkjet volume is 10pL, water phase ink is being used
When printing, since the surface tension of water is larger, printing surface needs to carry out hydrophilic treated, the oxide semiconductor printed after processing
Film dimensions are more than 80 μm, cannot meet the requirement of high integration.If reducing nozzle, reduces inkjet volume, then be easy to cause
Nozzle blocks;And the related process of current 1pL inkjet printings is also very immature, can not be applied to large area and prepare.
The method that surface modification usually may be used obtains the substrate surface of different contact angles, various sizes of to obtain
Ink jet printing oxide semiconductor thin-film array;But due to the droplet size substantially constant of ink-jet, oxide semiconductor thin-film ruler
Very little reduction will necessarily bring the increase of thickness.Experiment shows that oxide is partly led when the contact angle of substrate surface is more than 30 °
The size of body thin film can be reduced to 30 μm hereinafter, but its thickness will be greater than 100nm at this time, the thin-film transistor performance of preparation is very
Difference illustrates that thicker oxide semiconductor thin-film is unfavorable for preparing high performance thin film transistor (TFT).
Therefore, in view of the shortcomings of the prior art, proposing a kind of to have both small size and low thickness by printing technology to prepare
The method of oxide semiconductor thin-film is particularly necessary with overcome the deficiencies in the prior art.
Invention content
To solve the above-mentioned problems of the prior art, the present invention provides a kind of making sides of oxide semiconductor thin-film
Method, which effectively controls the size and thickness of oxide semiconductor thin-film simultaneously, so that the oxide semiconductor
When film is applied in oxide thin film transistor, it can ensure that the oxide thin film transistor obtains excellent properties.
In order to reach foregoing invention purpose, present invention employs the following technical solutions:
A kind of production method of oxide semiconductor thin-film, including:
Hydrophobic treatment is carried out to substrate, obtains modified substrate;
Prepare electric ink:Functional reagent is added into the precursor solution of oxide semiconductor, obtains electric ink;Its
In, the functional reagent has both hydrophily and improves viscosity effect;
The electric ink is printed on to the surface of the modified substrate, forms ink droplet;
After ink droplet drying, the ink droplet is made annealing treatment, oxide half is obtained on the modified substrate
Conductor thin film.
Further, the functional reagent is polyvinylpyrrolidone, the average molecular matter of the polyvinylpyrrolidone
Amount is 40000 or 1300000.
Further, when the functional reagent is the polyvinylpyrrolidone that relative molecular mass is 40000, described
The substance withdrawl syndrome of functional reagent in electric ink is 0.1mg/mL~0.5mg/mL;When the functional reagent is opposite point
When the polyvinylpyrrolidone that protonatomic mass is 1300000, the substance withdrawl syndrome of the functional reagent in the electric ink is
0.05mg/mL~0.5mg/mL.
Further, the contact angle of the modified substrate is 48 °~56 °.
Further, the precursor solution of the oxide semiconductor is the aqueous solution of metal nitrate.
Further, the aqueous solution of the metal nitrate includes In (NO3)3Aqueous solution, Ga (NO3)3Aqueous solution, Zn
(NO3)2At least one of aqueous solution.
Further, a concentration of 0.01mol/L~0.05mol/L of the precursor solution of the oxide semiconductor.
Further, the drying temperature of the ink droplet and annealing temperature are not less than 200 DEG C and are partly led not higher than oxide
The highest activation temperature of the presoma of body.
Further, the drying temperature of the ink droplet and annealing temperature are 200 DEG C~350 DEG C.
Another object of the present invention is to provide a kind of oxide thin film transistor, the oxide thin film transistor is to adopt
Use the oxide semiconductor thin-film that any production method as above obtains as active layer.
Another object of the present invention, which also resides in, provides a kind of production method of oxide thin film transistor, including:Dielectric layer
Making step, the making step of active layer, the making step of grid, source electrode and drain electrode making step;In the active layer
Making step in, using the dielectric layer as substrate, using the making side of as above any oxide semiconductor thin-film
Method.
Beneficial effects of the present invention:
(1) the present invention provides a kind of production method of completely new oxide semiconductor thin-film, by electric ink into
Row improves, and obtains a kind of mixed solution of the presoma of the oxide semiconductor of low concentration, thus passes through drying after printing
Annealing can be obtained the oxide semiconductor thin-film for having both small size and few thickness;As a result, on the substrate of same homalographic, compare
Production method in the prior art, you can make more oxide semiconductor thin-films, form highdensity oxide semiconductor
Membrane array;
(2) production method of oxide semiconductor thin-film according to the present invention is avoided using vacuum equipment and photoetching work
Skill effectively reduces cost of manufacture, while disclosure satisfy that prepared by the large area of industrialized production and requiring;
(3) production method based on oxide semiconductor thin-film provided by the invention, can be applied to sull
In transistor and its making, having in oxide thin film transistor is made using the production method of the oxide semiconductor thin-film
Active layer;The production method of middle active layer compared with prior art has both the oxide thin film transistor of small size and few thickness with this
As active layer, more oxide thin film transistors can be maximumlly integrated on unit area, to meet display backboard
High pixel demand;
(4) production method of oxide thin film transistor according to the present invention, oxide in used electric ink
The concentration concentration more in the prior art of the presoma of semiconductor is lower, print acquisition ink droplet it is annealed can be obtained thickness compared with
Few oxide semiconductor thin-film;At the same time, by controlling the concentration of the presoma of oxide semiconductor in the electric ink,
The thickness of i.e. controllable pre-prepared active layer, and the oxide semiconductor thin-film uniformity is higher, is more easy to obtain high performance
Oxide thin film transistor.
Description of the drawings
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing:
Fig. 1 is the optics pictorial diagram of according to an embodiment of the invention 1 oxide semiconductor thin-film array;
Fig. 2 is the film morphology figure of according to an embodiment of the invention 1 oxide semiconductor thin-film array;
Fig. 3 is the optics pictorial diagram of the oxide semiconductor thin-film array of comparative example 1 according to the present invention;
Fig. 4 is the film morphology figure of the oxide semiconductor thin-film array of comparative example 1 according to the present invention;
Fig. 5 is the optics pictorial diagram of the oxide semiconductor thin-film array of comparative example 2 according to the present invention;
Fig. 6 is the film morphology figure of the oxide semiconductor thin-film array of comparative example 2 according to the present invention;
Fig. 7 be according to an embodiment of the invention 1, the minimum of the oxide semiconductor thin-film array of comparative example 1, comparative example 2
Point spacing comparison diagram;
Fig. 8 be according to an embodiment of the invention 1, the thickness of the oxide semiconductor thin-film array of comparative example 1, comparative example 2
Comparison diagram;
Fig. 9 is the structural schematic diagram of 3 oxide thin film transistor according to an embodiment of the invention;
Figure 10 is the normalization transfer curve figure of 3 oxide thin film transistor according to an embodiment of the invention;
Figure 11 is the normalization transfer curve figure of 4 oxide thin film transistor according to an embodiment of the invention;
Figure 12 is the normalization transfer curve figure of the oxide thin film transistor of comparative example 3 according to the present invention;
Figure 13 be according to an embodiment of the invention 5 and embodiment 3 oxide thin film transistor normalization transfer curve
Comparison diagram.
Specific implementation mode
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to come in many different forms real
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, providing these implementations
Example is in order to explain the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.In the accompanying drawings, for the sake of clarity, element can be exaggerated
Shape and size, and identical label will be used to indicate same or analogous element always.
Term " first ", " second " etc. herein can be used to describe various substances although will be appreciated that, these
Substance should not be limited by these terms.These terms are only used to distinguish a substance with another substance.
Embodiment 1
Present embodiments provide a kind of production method of oxide semiconductor thin-film comprising following step:
S1, hydrophobic treatment is carried out to substrate, obtains modified substrate.
In general, after being cleaned up to substrate, it can be modified, that is, be carried out by hmds (abbreviation HMDS)
Silicic acid anhydride obtains the modified substrate that contact angle is 52 ° ± 4 °.
In the present embodiment, substrate has specifically selected the silicon chip of the thermal oxide silica containing 300nm thickness;Substrate its
Details are not described herein for his optional material, and those skilled in the art can refer to the prior art and be selected according to specific requirement.
S2, electric ink is prepared.
Specifically, functional reagent is added into the precursor solution of oxide semiconductor, obtains electric ink.Wherein,
The functional reagent has both hydrophily and improves viscosity effect, in this way, on the one hand the functional reagent can neutralize oxide semiconductor
Hydrophobic effect of the precursor solution in modified substrate, on the other hand can improve the electronics using its highly viscous characteristic
The viscosity of ink, and the fast shaping when forming ink droplet.
The functional reagent is preferably polyvinylpyrrolidone (abbreviation PVP), and the relative molecular mass of general common PVP is
40000 and 1,300,000 two kind, it is respectively referred to as PVP 40000 and PVP 1300000 below.
When functional reagent is specially PVP 40000, a concentration of 0.1mg/mL~0.5mg/mL in electric ink;When
When functional reagent is specially PVP 1300000, a concentration of 0.05mg/mL~0.5mg/mL in electric ink.
More specifically, the precursor solution of the oxide semiconductor is the aqueous solution of metal nitrate, preferably In
(NO3)3Aqueous solution, Ga (NO3)3Aqueous solution, Zn (NO3)2In aqueous solution any one or at least two mixed solution.
Usually, a concentration of 0.01mol/L~0.05mol/L of the precursor solution of control oxide semiconductor;In view of
The additive amount of functional reagent is seldom in electric ink, therefore the concentration of the presoma of oxide semiconductor and preparation in electric ink
The concentration variation of the precursor solution of oxide semiconductor before is little.In this way, in compared with prior art, in the electric ink
Oxide semiconductor presoma concentration it is relatively low, follow-up annealed processing can be obtained the smaller oxide semiconductor of thickness
Film.
In the present embodiment, a concentration of 0.1mg/mL of PVP 40000 and the forerunner of oxide semiconductor in electric ink
Liquid solution is the In (NO of 0.02mol/L3)3Aqueous solution.
S3, the surface that electric ink is printed on to modified substrate form ink droplet.
In the present embodiment, using 2831 type ink-jet apparatus of DM by above-mentioned electric ink ink jet printing in modified substrate
Surface;The temperature of the temperature and nozzle in printing process that are preferably provided with the modified substrate before printing is 40 DEG C or so.
S4, after ink droplet drying after, ink droplet is made annealing treatment, oxide semiconductor thin-film is obtained on modified substrate.
Usually, it controls the drying temperature of ink droplet and annealing temperature is not less than 200 DEG C and is not higher than oxide semiconductor
Presoma highest activation temperature;It is preferred that controlling in the range of 200 DEG C~350 DEG C.
In the present embodiment, it is dried and anneals respectively using 250 DEG C of thermal station and 250 DEG C of Muffle furnace.
On the one hand ink droplet can enable solvent volatilization removal therein, on the other hand wherein by dry and annealing
The presoma of oxide semiconductor be decomposed thermally to form oxide semiconductor in annealing, and the oxygen to be formed and be made in advance that forms a film
Compound semiconductive thin film.
Obviously, if foring several ink droplets by being printed on the surface of modified substrate, correspondence can make oxidation
Object semiconductor film membrane array.
Optics material object characterization and morphology characterization have been carried out respectively to the oxide semiconductor thin-film array that the present embodiment makes,
Its optics pictorial diagram and film morphology figure difference are as depicted in figs. 1 and 2.From Fig. 1 and Fig. 2 as can be seen that the present embodiment provides
Oxide semiconductor thin-film production method, obtain the oxide that lattice dimensions are 35 μm or so, thickness is 12nm or so
Semiconductor film membrane array, the index request for meeting small size, lacking thickness.
In order to further illustrate the technique effect of the production method of the oxide semiconductor thin-film of the offer of embodiment 1, carry out
Contrast experiment.
Comparative example 1
The printing condition of comparative example 1 uses method in the prior art, using substrate in the same manner as in Example 1, and
UV hydrophilic treateds have been carried out, have obtained contact angle close to 0 ° of hydrophobic substrate;Meanwhile with the oxide semiconductor of 0.1mol/L
Precursor solution is as ink;Remaining obtains the first comparison oxide semiconductor thin-film with reference to described in embodiment 1.
Optics material object characterization and morphology characterization are carried out respectively to the first comparison oxide semiconductor thin-film, optics is real
Object figure and film morphology figure difference are as shown in Figure 3 and Figure 4.As can be seen that the oxide that this comparative example provides from Fig. 3 and Fig. 4
The production method of semiconductive thin film obtains the first comparison oxide that lattice dimensions are 85 μm or so, thickness is 10nm or so
Semiconductor film membrane array, belong to a kind of large scale, few thickness oxide semiconductor thin-film.
It is worth noting that the concentration of the presoma of oxide semiconductor is compared with embodiment in ink used in this comparative example
Respective concentration in 1 is bigger, also only obtains the first comparison oxide semiconductor thin-film array that thickness is 10nm or so;It is aobvious
So, if taking the precursor solution such as the oxide semiconductor of same concentrations in embodiment 1 as ink, then due to its size
Larger, thickness will be less than 5nm.
Comparative example 2
The printing condition of comparative example 2 is used in the same manner as in Example 1 i.e. using improved method in the prior art
Modified substrate;Meanwhile only using in embodiment 1 with the precursor solution of the oxide semiconductor of concentration as ink;Remaining
With reference to described in embodiment 1, the second comparison oxide semiconductor thin-film is obtained.
Optics material object characterization and morphology characterization are carried out respectively to the second comparison oxide semiconductor thin-film, optics is real
Object figure and film morphology figure difference are as shown in Figure 5 and Figure 6.As can be known from Fig. 5 and Fig. 6, the oxide that this comparative example provides
The production method of semiconductive thin film obtains the second comparison oxide that lattice dimensions are 8 μm or so, thickness is 300nm or so
Semiconductor film membrane array, belong to a kind of small size, more thickness oxide semiconductor thin-film.
By the smallest point spacing of the oxide semiconductor thin-film array obtained in embodiment 1, comparative example 1 and comparative example 2
And thickness is compared respectively, comparison diagram is respectively as shown in 7 and Fig. 8.From Fig. 7 and Fig. 8 as can be seen that in different prints
Under the conditions of brush (being specially the hydrophilic/hydrophobic degree of substrate and the composition of electric ink), using the oxide in embodiment 1 half
The production method of conductor thin film can be such that smallest point spacing is reduced by 90 μm or so on the one hand by carrying out hydrophobic treatment to substrate
To 50 μm or so, the integrated level of oxide semiconductor thin-film array is greatly improved;On the other hand by adding function examination
Electric ink is prepared in agent, so that the thickness of oxide semiconductor thin-film is reduced to 12nm or so from 300nm or so.
Embodiment 2
In the description of embodiment 2, details are not described herein with the something in common of embodiment 1, only describes with embodiment 1 not
Same place.Embodiment 2 difference from example 1 is that, in step s 2, the concentration of PVP 1300000 in electric ink
In (the NO that precursor solution for 0.05mg/mL and oxide semiconductor is 0.02mol/L3)3Aqueous solution.
The oxide semiconductor thin-film array that the present embodiment obtains has and the oxide semiconductor thin-film battle array in embodiment 1
Arrange comparable optics pictorial diagram and film morphology figure.
Embodiment 3
The production method of the oxide semiconductor thin-film provided based on above-described embodiment 1 and embodiment 2 can make small
The oxide semiconductor thin-film of size, few thickness, can be applied in oxide thin film transistor field, using as therein
Active layer, to obtain high performance oxide thin film transistor.
Referring in particular to Fig. 9, oxide thin film transistor provided in this embodiment is bottom gate type;The oxide thin film transistor
Including lamination successively setting grid 11, dielectric layer 12, active layer 13, and be oppositely arranged on the active layer 13 both ends and
The source electrode 14 contacted with dielectric layer 12 and drain electrode 15.
Specifically, which is to be formed by the oxide semiconductor thin-film of small size, few thickness.
Hereinafter, the production method that will be described in detail the bottom gate type oxide thin film transistor (TFT) of the present embodiment;According to this implementation
The production method of the bottom gate type oxide thin film transistor (TFT) of example includes the following steps:
Q1, dielectric layer is made on grid.
In the present embodiment, grid and dielectric layer are all made of the silicon chip of the thermal oxide silica including 300nm thickness.
Q2, active layer is made on the dielectric layer.
Active layer is made on the dielectric layer, substantially using dielectric layer as a kind of substrate, therefore it need to be carried out first
Hydrophobic treatment is specifically modified the surface of thermal oxide silica by HMDS, its contact angle is increased to 52 ° ± 4 °, with
Modified substrate as the active layer made in advance.
Then electric ink is prepared.
Specifically, functional reagent is added into the precursor solution of oxide semiconductor, obtains electric ink.Wherein,
The functional reagent has both hydrophily and improves viscosity effect, in this way, on the one hand the functional reagent can neutralize oxide semiconductor
Hydrophobic effect of the precursor solution in modified substrate, on the other hand can improve the electronics using its highly viscous characteristic
The viscosity of ink, and the fast shaping when forming ink droplet.
The functional reagent is preferably PVP, and generally there are commonly 1,300,000 two kinds of PVP 40000 and PVP.
When functional reagent is specially PVP 40000, a concentration of 0.1mg/mL~0.5mg/mL in electric ink;When
When functional reagent is specially PVP 1300000, a concentration of 0.05mg/mL~0.5mg/mL in electric ink.
More specifically, the precursor solution of the oxide semiconductor is the aqueous solution of metal nitrate, preferably In
(NO3)3Aqueous solution, Ga (NO3)3Aqueous solution, Zn (NO3)2In aqueous solution any one or at least two mixed solution.
Usually, a concentration of 0.01mol/L~0.05mol/L of the precursor solution of control oxide semiconductor;In this way,
In compared with prior art, the concentration of the presoma of the oxide semiconductor in the electric ink is relatively low, and follow-up annealed processing is
The smaller oxide semiconductor thin-film of available thickness.
In the present embodiment, a concentration of 0.1mg/mL of PVP 40000 and the forerunner of oxide semiconductor in electric ink
Liquid solution is the In (NO of 0.02mol/L3)3Aqueous solution.
Finally, electric ink is printed on the dielectric layer through hydrophobic treatment and is formed ink droplet, after ink droplet drying, to ink
Drop is made annealing treatment, and active layer is obtained.
In the present embodiment, using 2831 type ink-jet apparatus of DM by above-mentioned electric ink ink jet printing in through hydrophobic treatment
Dielectric layer surface;The temperature of the temperature and nozzle in printing process that are preferably provided with the modification dielectric layer before printing is 40 DEG C
Left and right.
Usually, it controls the drying temperature of ink droplet and annealing temperature is not less than 200 DEG C and is not higher than oxide semiconductor
Presoma highest activation temperature;It is preferred that controlling in the range of 200 DEG C~350 DEG C.
In the present embodiment, it is dried and anneals respectively using 250 DEG C of thermal station and 250 DEG C of Muffle furnace.
On the one hand ink droplet can enable solvent volatilization removal therein, on the other hand wherein by dry and annealing
The presoma of oxide semiconductor be decomposed thermally to form oxide semiconductor in annealing, and form a film and form oxide and partly lead
Body thin film, using the active layer as the oxide thin film transistor made in advance.
Q3, source electrode and drain electrode is made respectively on active layer.
Using traditional microelectronic technique, such as magnetron sputtering molybdenum niobium alloy simultaneously uses stripping technology (abbreviation lift-off works
Skill) obtain the conducting channel that channel length is 10 μm.
In this way, completing the making of the bottom gate type oxide thin film transistor (TFT) in the present embodiment.Certainly, if as made
Top gate type oxide thin film transistor only need to change the manufacture craft of grid and change the production order of each structure sheaf, and
The making of active layer is not interfered with.
Active layer in the oxide thin film transistor made in view of the present embodiment has the characteristics that small size, few thickness,
Therefore, oxide thin film transistor can be more integrated on unit area, to meet height when it is applied to display backboard
Pixel demand.
Embodiment 4
In the description of embodiment 4, details are not described herein with the something in common of embodiment 3, only describes with embodiment 3 not
Same place.Embodiment 4 and embodiment 3 the difference is that, in the oxide thin film transistor of the present embodiment, wherein active
The functional reagent for including in layer is specially the PVP1300000 of 0.05mg/mL.
With the oxide thin film transistor in the present embodiment correspondingly, the system of the oxide thin film transistor of the present embodiment
Make the production method of the oxide thin film transistor of method and embodiment 3 the difference is that, in step Q2, electric ink
A concentration of 0.05mg/mL of middle PVP 1300000 and the In (NO that the precursor solution of oxide semiconductor is 0.02mol/L3)3
Aqueous solution.
In order to further illustrate active layer to the performance of oxide thin film transistor in above-described embodiment 3 and embodiment 4
It influences, has carried out contrast experiment.
Comparative example 3
Production method, that is, general the production method in the prior art for the oxide thin film transistor that this comparative example uses, i.e.,
When making active layer equally using dielectric layer as a kind of substrate, and the hydrophilic places UV are carried out to the surface of thermal oxide silica
Reason, so that its contact angle is close to 0 ° using the hydrophobic substrate as the active layer made in advance;Meanwhile only with embodiment 3, embodiment
Precursor solution in 4 with the oxide semiconductor of concentration is as ink;Remaining is obtained with reference to described in embodiment 3 and embodiment 4
Obtained comparison oxide thin film transistor.
The normalization transfer characteristic of the oxide thin film transistor in embodiment 3, embodiment 4, comparative example 3 is carried out respectively
It measures, normalization transfer curve is respectively as shown in Figure 10-Figure 12.Pass through comparison diagram 10- Figure 12, it can be seen that embodiment
3, the mobility of the oxide thin film transistor obtained in embodiment 4 and comparative example 3 is respectively 2.78cm2·V-1·s-1,
2.46cm2·V-1·s-1And 3.36cm2·V-1·s-1, illustrate brilliant using the sull in above-described embodiment 3, embodiment 4
The oxide thin film transistor performance that the production method of body pipe obtains is more preferable, and essence is in above-described embodiment 3, embodiment 4
Active layer is more easy to obtain high performance oxide thin film transistor compared with the active layer uniformity higher in comparative example 3.
Embodiment 5
It in the description of embodiment 5, repeats no more, only describes with embodiment 3 not again with the something in common of embodiment 3
Same place.Embodiment 5 and embodiment 3 the difference is that, in the oxide thin film transistor of the present embodiment, wherein active
The functional reagent for including in layer is specially the PVP 40000 of the PVP 40000 and 0.5mg/mL of 0.2mg/mL respectively.
With the two oxides thin film transistor (TFT) in the present embodiment correspondingly, the oxide thin film transistor of the present embodiment
Production method and embodiment 3 oxide thin film transistor production method the difference is that, in step Q2, electronics
Ink is respectively that the wherein precursor solution of a concentration of 0.2mg/mL of PVP 40000 and oxide semiconductor is 0.02mol/L
In (NO3)3Aqueous solution, and the wherein a concentration of 0.5mg/mL of PVP 40000 and the precursor solution of oxide semiconductor
For the In (NO of 0.02mol/L3)3Aqueous solution.
The normalization transfer characteristic of two oxides thin film transistor (TFT) in the present embodiment is determined, and is returned
The normalization transfer curve of one change transfer curve and the oxide thin film transistor in embodiment 3 is compared, such as Figure 13 institutes
Show.It can be observed from fig. 13 that the concentration with functional reagent in electric ink increases, the oxidation under equal conditions obtained
The electric current of object thin film transistor (TFT) is gradually reduced, and the device performance of oxide thin film transistor is gradually deteriorated;Usually, when function is tried
When agent uses PVP 40000, its a concentration of 0.1mg/mL~0.5mg/mL in electric ink is controlled.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (11)
1. a kind of production method of oxide semiconductor thin-film, which is characterized in that including:
Hydrophobic treatment is carried out to substrate, obtains modified substrate;
Prepare electric ink:Functional reagent is added into the precursor solution of oxide semiconductor, obtains electric ink;Wherein,
The functional reagent has both hydrophily and improves viscosity effect;
The electric ink is printed on to the surface of the modified substrate, forms ink droplet;
After ink droplet drying, the ink droplet is made annealing treatment, oxide semiconductor is obtained on the modified substrate
Film.
2. manufacturing method according to claim 1, which is characterized in that the functional reagent is polyvinylpyrrolidone, institute
The relative molecular mass for stating polyvinylpyrrolidone is 40000 or 1300000.
3. production method according to claim 2, which is characterized in that when the functional reagent is that relative molecular mass is
When 40000 polyvinylpyrrolidone, the substance withdrawl syndrome of the functional reagent in the electric ink be 0.1mg/mL~
0.5mg/mL;
When the functional reagent is the polyvinylpyrrolidone that relative molecular mass is 1300000, in the electric ink
Functional reagent substance withdrawl syndrome be 0.05mg/mL~0.5mg/mL.
4. production method according to claim 3, which is characterized in that the contact angle of the modified substrate is 48 °~56 °.
5. according to any production methods of claim 1-4, which is characterized in that the presoma of the oxide semiconductor is molten
Liquid is the aqueous solution of metal nitrate.
6. production method according to claim 5, which is characterized in that the aqueous solution of the metal nitrate includes In
(NO3)3Aqueous solution, Ga (NO3)3Aqueous solution, Zn (NO3)2At least one of aqueous solution.
7. production method according to claim 5, which is characterized in that the precursor solution of the oxide semiconductor it is dense
Degree is 0.01mol/L~0.05mol/L.
8. production method according to claim 5, which is characterized in that the drying temperature and annealing temperature of the ink droplet are not
The highest activation temperature of presoma less than 200 DEG C and not higher than oxide semiconductor.
9. production method according to claim 8, which is characterized in that the drying temperature and annealing temperature of the ink droplet be
200 DEG C~350 DEG C.
10. a kind of oxide thin film transistor, which is characterized in that the oxide thin film transistor is with using such as claim 1-
The oxide semiconductor thin-film that 9 any production methods obtain is as active layer.
11. a kind of production method of oxide thin film transistor, including:The making step of dielectric layer, the making step of active layer,
The making step of grid, the making step of source electrode and drain electrode;It is characterized in that, in the making step of the active layer, with institute
Dielectric layer is stated as substrate, using the production method of the oxide semiconductor thin-film as described in claim 1-9 is any.
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