CN108321261A - A kind of preparation method of graphical sapphire substrate - Google Patents
A kind of preparation method of graphical sapphire substrate Download PDFInfo
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- CN108321261A CN108321261A CN201810012156.XA CN201810012156A CN108321261A CN 108321261 A CN108321261 A CN 108321261A CN 201810012156 A CN201810012156 A CN 201810012156A CN 108321261 A CN108321261 A CN 108321261A
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- sapphire substrate
- etching
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
Abstract
A kind of preparation method of graphical sapphire substrate, includes the following steps：Step 1 cleans Sapphire Substrate；Step 2 forms a layer photoresist mask pattern in sapphire substrate surface；Sapphire Substrate with photoresist mask pattern is put into ICP dry etching equipments and performs etching operation by step 3, is each led into toward ICP dry etching equipments by BCl3Gas and CHF3Gas forms mixed gas, CHF in the mixed gas3The input flow rate and BCl of gas3The ratio value of the input flow rate of gas is less than 40% and is more than 0, and etching operation is made of main etching stage and over etching stage, and the main etching time is more than the over etching time, and graphical sapphire substrate is prepared.The effective solution of the present invention low problem of ICP equipment capacities, reduces the manufacturing cost of graphical sapphire substrate, improves the process rate of graphical sapphire substrate.
Description
Technical field
The invention belongs to technical field of semiconductor preparation, specifically a kind of preparation side of graphical sapphire substrate
Method.
Background technology
Iii-v gallium nitride（GaN）Base LED component shows in semiconductor lighting, outdoor large screen, backlight, vehicle head
The application fields such as lamp are used widely.However, it is always device light emitting efficiency and cost to receive LED industry focus of attention.
In LED industry chain link, upstream substrate material directly affects the developing direction of middle and lower reaches extension, chip, encapsulation technology.By
Technical maturity and comprehensive cost performance decision, graphical sapphire substrate（Patterned Sapphire Substrates, letter
Claim PSS）Have become the mainstream substrate material of GaN base LED epitaxial growths.
PSS substrates mainly use photoetching process binding plasma（ICP）Dry etching technology is on a sapphire substrate
It prepares and realizes.PSS preparation process flows mainly include the following steps：First, sapphire plain film substrate is cleaned, spin coating,
Nikon Stepper step printings and developing process form cylindric mask pattern array on plane sapphire substrate surface；
Then, using ICP equipment dry etching sapphires, and mask is removed, microstructure graph array is formed in sapphire surface, to
Realize prepared by PSS.There are two severe technological challenges in PSS batch productions.First technological challenge is the Huang of PSS processing procedures
Light technology uses second-hand Nikon Stepper used equipments, the stability of the equipment to be influenced big, mask by photoresist mask thicknesses
Thicker, equipment operation stability is poorer.Second technological challenge is that, due to sapphire material extreme hardness, hardness is only second to
Diamond hardness, there are etch rates during ICP dry etchings for sapphire slowly, sapphire is low to the etching selection ratio of mask
The problem of.Traditional sapphire lithographic technique generally uses pure boron chloride（BCl3）As etching gas, as shown in Fig. 2, ICP
The working range of lower electrode power is the W of 100 W -800, the corresponding etch rate ranging from nm/min of 25 nm/min -90,
And etching selection ratio drops to 0.3 from 0.85, etch rate and the etching selection ratio of sapphire material are the contradiction mutually restricted
Body.Improve etch rate, it will reduce etching selection ratio, lead to PSS off-gauge product requirements, and reduce etch rate, then
ICP equipment capacities are influenced, PSS production costs are increased.
Currently, traditional PS S technologies of preparing are probably to go to carry out PSS process optimizations and procedure for producing stabilization from two directions.
On the one hand it is to start with from yellow light technique, PSS microstructure graph sizes is improved by improving photoresist mask thicknesses, to reach
The specification requirement of PSS products, but the increase of photoresist mask thicknesses will certainly make Stepper stabilization of equipment performance be deteriorated, exposure technology
Windows narrow causes production yield to decline, and manufacturing cost is caused to increase；On the other hand, start with from ICP etching technics, pass through drop
The lower electrode power of low ICP increases etching selection ratio of the sapphire to mask, but lower electrode power reduces while reducing indigo plant
The etch rate of jewel causes ICP equipment capacities further to decline.It is carried in addition, increase PSS pattern heights are that industrial circle is generally acknowledged
Rise the most effective approach of LED light extraction efficiency.But PSS pattern heights are promoted, the procedure for producing of PSS will certainly be further decreased
Yield increases production cost, is unfavorable for the reduction of LED industry overall cost.How to solve in PSS preparation process etch rate with
The technical bottleneck that etching selection ratio mutually restricts is always the generally acknowledged international technical barrier of industrial circle.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation methods of graphical sapphire substrate, solve ICP
The low problem of equipment capacity, reduces the manufacturing cost of graphical sapphire substrate, improves the system of graphical sapphire substrate
Journey yield.
In order to solve the above-mentioned technical problem, the present invention takes following technical scheme：
A kind of preparation method of graphical sapphire substrate, includes the following steps：
Step 1 cleans Sapphire Substrate；
Step 2 forms a layer photoresist mask pattern in sapphire substrate surface；
Sapphire Substrate with photoresist mask pattern is put into ICP dry etching equipments and performs etching operation by step 3,
BCl is each led into toward ICP dry etching equipments3Gas and CHF3Gas forms mixed gas, CHF in the mixed gas3Gas
Flow and BCl3The ratio value range of gas flow is in 0-40%.Meanwhile it being passed through He gas in tray bottom, in etching process
Sapphire Substrate is cooled down, etching operation is made of main etching stage and over etching stage, and the main etching time was more than quarter
The time is lost, graphical sapphire substrate is prepared.
The BCl being passed through in ICP dry etching equipments in the step 33Gas flow ranging from 50 sccm-120
sccm, CHF3Gas flow ranging from 0 sccm-40 sccm, CHF3/BCl3Gas flow ratio ranging from 0-40%, wherein greatly
In 0.
Upper electrode power is 1000-1500W, lower electrode power 200- in ICP dry etching equipments in the step 3
800W, the wherein lower electrode power in main etching stage are 200-700W, and the main etching time accounts for the 60%-80% of total etch period, mistake
The lower electrode power of etch stages ranging from 700-800W, over etching time account for the 20%-40% of total etch period.
The internal pressure modification scope of ICP dry etching equipments is 1.5mT-5mT in the step 3.
It is also cooled down after the completion of etching in the step 3, the modification scope of cooling temperature is -20 DEG C -40 DEG C, and ICP is dry
Control ranging from 3T-8T is emphasized in He air pressures in method etching apparatus,.
The step 1 specifically includes：Sapphire Substrate is put into the concentrated sulfuric acid and soaking and washing in hydrogen peroxide mixed solution,
The volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 5:1-3:1, for the control of mixed solution temperature at 100 DEG C -150 DEG C, scavenging period is 10 points
Clock -30 minutes.
The dimensions of Sapphire Substrate in the step 1 is 2 inches, 4 inches or 6 inches.
The step 2 specifically includes：Photoresist mask layer is coated in sapphire substrate surface, using spin coating or spraying side
Formula is coated, and the thickness of photoresist mask layer is 1.0 μm -10 μm；Then to the Sapphire Substrate with photoresist mask layer
Step printing is carried out, after developed, obtains the Sapphire Substrate with photoresist mask pattern.
The period of photoresist mask pattern after developing in the step 2 is 1.0 μm -10 μm, photoresist mask pattern bottom
Diameter is 0.75 μm -9 μm, and pattern height is 0.95 μm -9.9 μm.
Photoresist mask pattern pattern after developing in the step 2 is cylindric, round table-like or rounding mesa-shaped.
The invention has the advantages that：
（1）Effective solution ICP equipment capacities low problem.By optimizing CHF3/BCl3Gas ratio is obviously improved blue treasured
Stone is to the etching selection ratio of photoresist mask, to which entire ICP etching processes can be in high lower electrode power（＞ 600W）Under
It carries out, sapphire etch rate is maintained at 80 nm/min or more, and the etching process of entire PSS foreshortened within 35 minutes, significantly
The output of ICP equipment is improved, the ICP equipment capacities under new technology promote 30% or more with respect to the production capacity under conventional etch techniques,
Play the effect for substantially reducing PSS manufacturing costs；
（2）The thickness for further decreasing photoresist mask, to increase the process window of Stepper step printings, raising is set
Standby stability, promotes PSS process rates, to be conducive to further control the manufacturing cost of PSS；
（3）Under the premise of relatively low mask thicknesses and shorter ICP etch periods, the uniformity of PSS products is significantly improved, maximum
Promote to degree PSS product quality so that PSS products have the bigger market competitiveness.
Description of the drawings
Attached drawing 1 is preparation process flow schematic diagram of the present invention；
Attached drawing 2 is under the conditions of traditional sapphire lithographic technique, sapphire etch rate and sapphire is to photoresist mask etching
The graph of relation that selection ratio changes with lower electrode power；
Attached drawing 3 is the CHF of the present invention3/BCl3Under secondary mask etching technical conditions, etch by-products are redeposited in sapphire
The SEM image on surface；
Attached drawing 4 is the CHF of the present invention3/BCl3Under secondary mask etching technical conditions, when lower electrode power is 700W, Lan Bao
Stone etch rate and sapphire select ratio with CHF photoresist mask etching3/BCl3Mixed gas flow is more bent than the relationship of variation
Line chart；
The schematic diagram that attached drawing 5 is the photoresist mask pattern that is prepared of the present invention when being cylinder；
Attached drawing 6 is the PSS product schematic diagrames that the present invention is prepared.
Specific implementation mode
For that can further appreciate that the feature, technological means and the specific purposes reached, function of the present invention, with reference to
Present invention is further described in detail with specific implementation mode for attached drawing.
As shown in Fig. 1, a kind of preparation method of graphical sapphire substrate, includes the following steps：
Step 1 cleans Sapphire Substrate 1.The dimensions of Sapphire Substrate is 2 inches, 4 inches or 6 inches.It will
Sapphire Substrate is put into soaking and washing in the concentrated sulfuric acid and hydrogen peroxide mixed solution, and the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 5:1-3:
1, for the control of mixed solution temperature at 100 DEG C -150 DEG C, scavenging period is -30 minutes 10 minutes.
Step 2 forms a layer photoresist mask pattern 2 on 1 surface of Sapphire Substrate.Specially：In Sapphire Substrate table
Face coats photoresist mask layer, is coated using spin coating or spraying method, and the thickness of photoresist mask layer is 1.0 μm -10 μm；
Then step printing is carried out to the Sapphire Substrate with photoresist mask layer, after developed, obtain and carry photoresist mask
The Sapphire Substrate of figure.The period of photoresist mask pattern after development is 1.0 μm -10 μm, photoresist mask pattern bottom diameter
It it is 0.75 μm -9 μm, pattern height is 0.95 μm -9.9 μm.And photoresist mask pattern pattern is cylindric, round table-like or falls
It is round table-like.
Sapphire Substrate with photoresist mask pattern is put into ICP dry etching equipments and performs etching by step 3
Operation is each led into toward ICP dry etching equipments by BCl3Gas and CHF3Gas forms mixed gas, and is passed through He gas, with
Substrate slice in etching process is cooled down.It needs to adjust suitable etching parameters and behaviour is performed etching to Sapphire Substrate
Make.Etching parameters include CHF3/ BCl3The flow-rate ratio of mixed gas, chamber pressure, upper/lower electrode power, helium（He）Pressure,
Cooling temperature and etch period.CHF in mixed gas3Gas flow and BCl3The ratio value of gas flow ranging from 0-40%,
CHF3/ BCl3Mixed gas total flow ranging from 50-120 sccm, etching operation is by main etching stage and over etching stage structure
At the main etching time is more than the over etching time, and graphical sapphire substrate is prepared.
Upper electrode power is 1000-1500W, lower electrode power 200- in ICP dry etching equipments in the step 3
800W, the wherein lower electrode power in main etching stage are 200-700W, and the main etching time accounts for the 60%-80% of total etch period, mistake
The lower electrode power of etch stages ranging from 700-800W, over etching time account for the 20%-40% of total etch period.ICP dry method is carved
Control ranging from 3T-8T is emphasized in He air pressures in erosion equipment, and the internal pressure modification scope of ICP dry etching equipments is 1.5mT-
5mT.The modification scope of cooling temperature is -20 DEG C -40 DEG C.
As shown in figure 3, in BCl3A certain proportion of CHF is mixed into gas3Gas, CHF3Gas makes during dry etching
By-product redeposit on the sidewall surfaces in spacing area and sapphire graphical between the top of mask, mask pattern.Mask
The by-product at top plays the effect of secondary mask, and being equivalent to reduces photoresist etch rate；The CH- of spacer region by-product at
Divide and reacted with sapphire O- ingredients, is conducive to promote sapphire etch rate to a certain extent, and on sapphire graphical side wall
By-product then can be final to PSS figure pattern rise regulating and controlling effect.As shown in figure 4, under the conditions of 700W lower electrode powers, it is blue
Jewel etch rate is with etching selection ratio with CHF3/BCl3The change curve of gas flow ratio, it is not difficult to find that working as CHF3/BCl3Gas
Body flow-rate ratio is 1:When 5, sapphire is more than 1.2 to the etching selection ratio of photoresist mask, and in sapphire selection than ＞'s 1
Under the premise of, sapphire etch rate remains to reach 80 nm/min or more.
Embodiment 1
Step 1：4 cun of sapphire plain film substrates are cleaned.Specially：By 4 cun of sapphire plain film substrates be put into the concentrated sulfuric acid with
The volume ratio of soaking and washing in hydrogen peroxide mixed solution, the concentrated sulfuric acid and hydrogen peroxide is 5:1, mixed solution temperature is controlled at 135 DEG C,
Scavenging period is 30 minutes.
Step 2：Using the semiconductor yellow light technique of standard, in 4 cun of sapphire plain film substrate surface one layer of AZ601 types of spin coating
Number photoresist mask layer, the thickness of mask layer is 2.25 μm ± 0.05 μm.Then Nikon Stepper step printings are used
Equipment is exposed Sapphire Substrate, and the reticle figure period of exposure is 3.0 μm ± 0.02 μm, mask diameter and spacing
Specification is 1 μm of 2 μ m.After developing to the sapphire plain film substrate after exposure, light is obtained in sapphire plain film substrate surface
Photoresist mask pattern array, as shown in figure 5, photoresist mask pattern pattern is cylinder, upper bottom diameter, the bottom diameter of mask pattern
It it is respectively 2.00 μm ± 0.05 μm, 2.05 μm ± 0.05 μm and 2.20 μm ± 0.05 μm with height.
Step 3：Sapphire plain film substrate with photoresist mask pattern is loaded into ICP and etches dedicated pallet apparatus
On, then pallet apparatus is put into ICP equipment cavities and carries out vacuumize process.Be arranged ICP etching parameters, parameter it is specific
Setting is as shown in table 1 below.After main etching and over etching process, take out sapphire substrate sheet from ICP cavitys, and to its into
After row cleaning treatment, it is the PSS products that 3 microns of specifications are 2.70 μm of 1.75 μ m to realize the period, as shown in Figure 6.
Etching menu setting prepared by 1,4 cun of PSS of table
| Parameter | Upper electrode power/W | Lower electrode power/W | BCl3Flow/sccm | CHF3Flow/sccm | Chamber pressure/mT | He air pressures are strong/T | Cooling temperature/DEG C | Etch period/min |
| Main etching | 1400 | 700 | 100 | 20 | 2.4 | 6 | 10 | 20 |
| Over etching | 1400 | 750 | 80 | 0 | 2.2 | 6 | 10 | 10 |
For the PSS products of 1.75 μ m, 2.70 μm of specifications, we compared conventional etch techniques and lithographic technique of the present invention
Two sets of key process parameters, as shown in table 2 below.It is not difficult to find that the present invention is based on CHF3/BCl3Secondary mask plasma dry
The PSS substrates technology of preparing of etching can improve the etch rate of sapphire material, while also can improve sapphire to photoresist
Etching selection ratio solves the problems, such as the technical bottleneck that etch rate is mutually restricted with etching selection ratio in PSS preparation process.
Table 2, conventional etch techniques and two sets of key process parameter contrast tables of lithographic technique of the present invention
| Parameter | Lower electrode power/W | BCl3Flow/sccm | CHF3Flow/sccm | He air pressures are strong/T | Cooling temperature/DEG C | Etch period/min | Sapphire etch rate | Sapphire selects ratio to photoresist |
| Traditional technology | 350 | 120 | 0 | 4 | 30 | 32min | 52 | 0.83 |
| The technology of the present invention | 700 | 100 | 20 | 6 | 10 | 20 min | 82 | 1.2 |
It should be noted that these are only the preferred embodiment of the present invention, it is not intended to restrict the invention, although with reference to reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to previous embodiment
Recorded technical solution is modified or equivalent replacement of some of the technical features, but all the present invention's
Within spirit and principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphical sapphire substrate, includes the following steps：
Step 1 cleans Sapphire Substrate；
Step 2 forms a layer photoresist mask pattern in sapphire substrate surface；
Sapphire Substrate with photoresist mask pattern is put into ICP dry etching equipments and performs etching operation by step 3,
BCl is each led into toward ICP dry etching equipments3Gas and CHF3Gas forms mixed gas, CHF in the mixed gas3Gas
Flow and BCl3The ratio value range of gas flow in 0-40%, meanwhile, He gas is passed through in tray bottom, in etching process
Sapphire Substrate is cooled down, etching operation is made of main etching stage and over etching stage, and the main etching time was more than quarter
The time is lost, graphical sapphire substrate is prepared.
2. the preparation method of graphical sapphire substrate according to claim 1, characteristic are, in the step 3
The BCl inputted in ICP dry etching equipments3Gas flow ranging from 50 sccm-120 sccm, CHF3Gas flow is 0
sccm-40 sccm, CHF3/BCl3Gas input flow amount is than ranging from 0-40%.
3. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that in the step 3
Upper electrode power is 1000-1500W, lower electrode power 200-800W, wherein main etching stage in ICP dry etching equipments
Lower electrode power is 200-700W, and the main etching time accounts for the 60%-80% of total etch period, the lower electrode power model in over etching stage
It encloses for 700-800W, the over etching time accounts for the 20%-40% of total etch period.
4. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that in the step 3
The internal pressure modification scope of ICP dry etching equipments is 1.5mT-5mT.
5. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that carved in the step 3
It is cooled down during erosion, the modification scope of cooling temperature is -20 DEG C -40 DEG C, the He air pressures in ICP dry etching equipments
Emphasize control ranging from 3T-8T.
6. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that the step 1 is specific
Including：Sapphire Substrate is put into the concentrated sulfuric acid and soaking and washing in hydrogen peroxide mixed solution, the volume ratio of the concentrated sulfuric acid and hydrogen peroxide
It is 5:1-3:1, for the control of mixed solution temperature at 100 DEG C -150 DEG C, scavenging period is -30 minutes 10 minutes.
7. the preparation method of graphical sapphire substrate according to claim 5, which is characterized in that in the step 1
The dimensions of Sapphire Substrate is 2 inches, 4 inches or 6 inches.
8. the preparation method of graphical sapphire substrate according to claim 6, which is characterized in that the step 2 is specific
Including：Photoresist mask layer is coated in sapphire substrate surface, is coated using spin coating or spraying method, photoresist mask layer
Thickness be 1.0 μm -10 μm；Then step printing is carried out to the Sapphire Substrate with photoresist mask layer, after developed,
Obtain the Sapphire Substrate with photoresist mask pattern.
9. the preparation method of graphical sapphire substrate according to claim 7, which is characterized in that shown in the step 2
The period of the photoresist mask pattern of movie queen is 1.0 μm -10 μm, and photoresist mask pattern bottom diameter is 0.75 μm -9 μm, and figure is high
Degree is 0.95 μm -9.9 μm.
10. the preparation method of graphical sapphire substrate according to claim 8, which is characterized in that in the step 2
Photoresist mask pattern pattern after development is cylindric, round table-like or rounding mesa-shaped.
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| CN113257970A (en) * | 2021-07-15 | 2021-08-13 | 广东中图半导体科技股份有限公司 | Patterned substrate for LED growth, epitaxial wafer and preparation method |
| CN114220893A (en) * | 2021-12-17 | 2022-03-22 | 北京北方华创微电子装备有限公司 | Etching method of sapphire substrate |
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