CN106017385A - Preparation method of step height standard sample block with nominal height ranging from 10 mu m to 100 mu m - Google Patents
Preparation method of step height standard sample block with nominal height ranging from 10 mu m to 100 mu m Download PDFInfo
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- CN106017385A CN106017385A CN201610578470.5A CN201610578470A CN106017385A CN 106017385 A CN106017385 A CN 106017385A CN 201610578470 A CN201610578470 A CN 201610578470A CN 106017385 A CN106017385 A CN 106017385A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
- G01B21/04—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness by measuring coordinates of points
- G01B21/042—Calibration or calibration artifacts
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
- G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
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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
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
Abstract
The invention discloses a preparation method of a step height standard sample block with nominal height ranging from 10 mu m to 100 mu m, and the preparation method belongs to the technical field of step profiler calibration. The preparation method comprises the steps of: adopting a double-side polished silicon wafer as a substrate material; growing an oxidation layer on the surface of the silicon wafer; painting a photoresist on the surface of oxidation layer; exposing, wherein a mask plate is negative plate, and a graphic region is a light-transmitting region; removing the photoresist from the light-transmitting region; adopting a reactive ion etching machine for etching, and etching the oxidation layer in a step region which is not masked by the photoresist away; adopting a deep reactive ion etching machine for etching the silicon wafer, and etching the silicon wafer in the step region which is not masked by the photoresist, wherein the etching depth is less than the nominal height of the standard sample block to be prepared; removing the photoresist; carrying out wet etching, wherein the etching depth reaches the requirement of the nominal height; and sputtering a metal protective layer on the surface of the silicon wafer, so as to prepare the desired standard sample block. The preparation method can accurately control the step height, meets the requirements of the standard sample block, and is low in cost.
Description
Technical field
The invention belongs to step instrument collimation technique field, particularly relate to the preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block.
Background technology
The test problem of a large amount of shoulder height is related to during integrated circuit and micro electronic mechanical system (MEMS) processing technology, the accurate measurement to step parameter, it is to ensure that the important means of device quality.At present, in semicon industry, shoulder height is measured by main use step instrument, and wherein the measuring method of step instrument mainly has: contact type measurement method and optical measuring method.Regardless of the step instrument of type, it is measured parameter and is the height value in samples vertical direction.Finding shows: China has thousand of of various step class measuring instruments, and this quasi-instrument is widely used in research and production unit, and the popularity rate of instrument is the highest.In order to ensure that step instrument obtains accurate data in the range of gamut, it should use a series of standard step height sample block consistent with step instrument range that step instrument is calibrated.
External VLSI has the standard step height sample block of micron dimension, use mask plate as substrate, use dry etch process to prepare step standard sample, the sample block depth of parallelism prepared by the method, have good uniformity, roughness is little, it is possible to meet the demand of semicon industry calibration step class measuring instrument.But, use mask plate to prepare step sample block processing technique as substrate complicated, cost is high.The domestic shoulder height sample block not having micron dimension, the step of altitude range 10 μm-100 μm uses two gauge block lapping-ins on optical flat to obtain, but the step accuracy obtained is low, step is discontinuous, roughness is poor, it is impossible to meet semicon industry demand.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block, can accurately control shoulder height, meets the requirement as standard sample, and low cost.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block, comprises the steps:
(1) use the silicon wafer of twin polishing as backing material, clean, be dried；
(2) oxide layer is grown at silicon wafer surface；
(3) at oxide layer surface resist coating, baking；
(4) by deep UV exposure, wherein mask plate is egative forme, and graphics field is transparent area；
(5) develop in aqueous slkali, remove the photoresist of transparent area, then toast；
(6) use reactive ion etching machine to perform etching, the oxide layer not having the stepped area of photoresist masking is etched away；
(7) using deep reaction ion etching machine engraving erosion silicon wafer, perform etching the silicon wafer of the stepped area not having photoresist masking, etching depth is less than the nominal height of standard sample to be prepared；
(8) acetone soln is used to remove photoresist；
(9) wet etching: the silicon wafer of the stepped area not having oxide layer to shelter is proceeded etching；Etching depth reaches nominal height requirement, and etching terminates, cleaning silicon chip；
(10) at silicon wafer surface splash-proofing sputtering metal protective layer, desired standard sample is prepared.
In step (1), first use acid electronic cleaning agent, then with deionized water ultrasonic cleaning 10-20 minute, then use alkalescence electronic cleaning agent, then with deionized water ultrasonic cleaning 10-20 minute, dry 10-20 minute afterwards；Wherein the order of acid electronic cleaning agent and alkalescence electronic cleaning agent is interchangeable.
In step (2), using thermal oxidation technology growth oxide layer, the thickness of oxide layer is 400
nm-500nm。
In step (2), thermal oxidation technology is dry-oxygen oxidation+wet-oxygen oxidation+dry-oxygen oxidation, the method that wherein wet oxygen uses hydrogen-oxygen synthesis.
In step (3), thickness 3 μm-4 μm of photoresist, toast 5-15 minute at a temperature of 100-150 DEG C.
In step (5), develop in NaOH solution, remove the photoresist of transparent area, then toast 5-15 minute at a temperature of 100-150 DEG C.
In step (6), etching gas is CHF3, etch rate is 120-160nm/min.
In step (7), etching depth is the nominal height μm that subtracts 5, and etching gas is SF6And C4F8, etch rate is set as 4 μm/min-5 μm/min.
In step (9), silicon wafer being placed in the Tetramethylammonium hydroxide corrosive liquid that concentration is 47%, perform etching the silicon wafer of the stepped area not having oxide layer to shelter, etch rate is 1 μm/min；Etching terminates to use ultrasonic cleaning silicon chip.
In step (10), coat of metal is crome metal, and thickness is 80 nm
-100nm。
Use and have the beneficial effects that produced by technique scheme: the present invention uses silicon wafer as substrate, uses deep reaction ion etching technique to prepare step, when etching depth is close to nominal height, then uses wet-etching technology that bench floor is carried out smooth treatment.The shoulder height sample block prepared by this etching technics, can accurately control step height dimension, the surface roughness that can obtain again and step side perpendicularity, meets the requirement as standard sample.
Accompanying drawing explanation
Fig. 1 is the structure chart of step one of the present invention；
Fig. 2 is the structure chart of step 2 of the present invention；
Fig. 3 is the structure chart of step 3 of the present invention；
Fig. 4 is the structure chart of step 4 of the present invention；
Fig. 5 is the structure chart of step 5 of the present invention；
Fig. 6 is the structure chart of step 6 of the present invention；
Fig. 7 is the structure chart of step 7 of the present invention；
Fig. 8 is the structure chart of step 8 of the present invention；
Fig. 9 is the structure chart of step 9 of the present invention；
Figure 10 is the structure chart of step 10 of the present invention；
Figure 11 is sample block stability assessment datagram of the present invention；
Figure 12 is the schematic diagram figure of the silicon wafer prepared；
Figure 13 is the schematic diagram that the silicon wafer prepared is divided into standard sample；
Figure 14 is the structure chart of the single standard sample prepared；
In figure: 1, silicon wafer；2, oxide layer；3, photoresist；4, coat of metal.
Detailed description of the invention
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
The present invention proposes a kind of use semiconductor etching process, with silicon chip as substrate, the method preparing 10 μm-100 μm standard step height sample blocks: use silicon wafer as substrate, deep reaction ion etching (DRIE etches-Deep reactive ion etching) technique is used to prepare step, when etching depth is close to desired size, then use wet-etching technology that bench floor is carried out smooth treatment.The shoulder height sample block prepared by this etching technics, can accurately control step height dimension, and the surface roughness that simultaneously can obtain and step side perpendicularity meet the requirement as standard substance.
The preparation method of the present invention a kind of nominal height 10 μm-100 μm standard step height sample block, comprises the steps:
(1) use the silicon wafer 1 of twin polishing as backing material, clean, be dried；
(2) in silicon wafer 1 superficial growth oxide layer 2；
(3) at oxide layer 2 surface resist coating 3, baking；
(4) by deep UV exposure, wherein mask plate is egative forme, and graphics field is transparent area；
(5) develop in aqueous slkali, remove the photoresist 3 of transparent area, then toast；
(6) use reactive ion etching machine to perform etching, the oxide layer 2 of the stepped area not having photoresist 3 to shelter is etched away；
(7) using deep reaction ion etching machine engraving erosion silicon wafer 1, perform etching the silicon wafer 1 of the stepped area not having photoresist 3 to shelter, etching depth is less than the nominal height of standard sample to be prepared；
(8) acetone soln is used to remove photoresist 3；
(9) wet etching: the silicon wafer 1 of the stepped area not having oxide layer to shelter is proceeded etching；Etching depth reaches nominal height requirement, and etching terminates, cleaning silicon chip；
(10) at silicon wafer 1 surface splash-proofing sputtering metal protective layer 4, desired standard sample is prepared.
Below by concrete data parameters, the preparation process further illustrating the present invention is as follows:
(1) using the silicon wafer of twin polishing as backing material, the crystalline phase of silicon wafer is 100；Successively use two kinds of different electronic cleaning agents of soda acid, deionized water ultrasonic cleaning 15 minutes, afterwards drying 15 minutes, as shown in Figure 1.Wherein, the solution that acid electronic cleaning agent is made up of deionized water, 30% hydrogen peroxide, 25% ammonia 14:3:1 by volume.The solution that alkalescence electronic cleaning agent is made up of deionized water, 30% hydrogen peroxide, 36% hydrochloric acid 7:1:1 by volume, such combination can be washed different impurity off, clean up thoroughly；
(2) using the oxide layer 2 of thermal oxidation technology growth 460nm, concrete technology is dry-oxygen oxidation+wet-oxygen oxidation+dry-oxygen oxidation, the method that wherein wet oxygen uses hydrogen-oxygen synthesis, as shown in Figure 2；
(3) it is coated with 3 μm-4 μm photoresists 3 at silicon chip surface, baking 10 minutes at a temperature of 120 DEG C, as shown in Figure 3；
(4) by deep UV exposure, wherein mask plate is egative forme, and graphics field is transparent area, as shown in Figure 4；
(5) develop in NaOH solution, remove the photoresist of transparent area, then baking 10 minutes at a temperature of 120 DEG C, as shown in Figure 5；
(6) using reactive ion etching machine to perform etching, the oxide layer not having the stepped area of photoresist masking etched away, etching gas is CHF3, etch rate is 150nm/min, and etching speed is fast, as shown in Figure 6；
(7) use deep reaction ion etching machine etching silicon wafer, the silicon chip of the stepped area not having photoresist masking is performed etching, as it is shown in fig. 7, etching gas is SF6And C4F8, namely it is passed through SF simultaneously6And C4F8, SF6Primarily serve the effect of etching, C4F8Being polymer protective effect, etch rate is set as 4 μm/min-5 μm/min, and etching depth is the calibrated altitude of standard sample the to be prepared μm that subtracts 5；
(8) acetone soln is used to remove photoresist, as shown in Figure 8；
(9) wet etching: as it is shown in figure 9, silicon chip to be placed into the Tetramethylammonium hydroxide ((CH that concentration is 47%3)4N(OH)·5H2O) in corrosive liquid, the silicon chip of the stepped area not having oxide layer to shelter being proceeded etching, etching depth reaches nominal height, and etch rate is 1 μm/min；Etching terminates to use ultrasonic cleaning silicon chip；
(10) at silicon chip surface splash-proofing sputtering metal chromium, sputtering thickness is 90nm, as shown in Figure 10.
The silicon wafer prepared is as shown in figure 12, in order to easy to use, after having prepared, silicon wafer is carried out scribing arrangement, the silicon wafer of one six cun is divided into the square-like block as shown in fig. 13 that of more than 100 10mm × 10mm, then it is fixed on the quartzy pedestal of 25mm × 25mm × 3mm, as shown in figure 14.Same silicon wafer can prepare more than 100 the identical sample block of shoulder height, namely shoulder height has identical structure, identical size, identical depth of groove.
Wherein, the height of step is controlled by etching technics, and the length of etch period determines the height of step.A series of sample blocks of differing heights to use multiple wafer to prepare, and by parameters such as the times that regulation etches, the time that each silicon wafer etching is different, thus can prepare the sample block of a series of differing heights.After sample block etching terminates, use step instrument that the shoulder height of sample block is measured, controlled the concrete height of step by measurement result.If the sample block of preparation is not reaching to expection height, then the parameter adjusting etching is needed again to prepare.
Height through wet method backward step has reached desired depth.The effect of splash-proofing sputtering metal chromium has two: one to be to protect sample block; after wet method terminates; the bottom surface of the step obtained is silicon; upper surface is silicon dioxide, and silicon is oxidizable, the most exposed in atmosphere; the silicon generation oxidation reaction of bottom surface; to gradually change the height of step, as standard substance, the stability of sample block will can not get ensureing；Two scope of applications being to increase sample block, step instrument includes contact pin type and optical profile type two kinds, optics step instrument measurement has certain limitation, the semipermeable membranes such as silicon dioxide cannot be measured, the sample block of preparation would be unavailable for the calibration of optics step instrument, after sputtering layer of metal chromium, avoid the limitation that optics step instrument is measured, extend the range of sample block.Due to coat of metal be on sample block uniform fold one layer as shown in Figure 10, namely the step upper and lower surface of sample block increases identical height, therefore after splash-proofing sputtering metal chromium, does not interferes with the shoulder height of sample block.
After prepared by sample block, using white light interferometer or nano-measuring machine with laser measurement function to calibrate sample block, both instruments can be traceable to optical maser wavelength, illustrates that the measured value of instrument is accurately.The nominal height such as preparing sample block is 10 μm, and the result of calibration is 9.95 μm, then then step instrument is calibrated by 9.95 μm as standard value.This sample block is measured, it is assumed that the result that step instrument is measured is 10.50 μm, then the step instrument measurement error when measuring the step about height 10 μm is 10.50 μm-9.95 μm=0.55 μm with step instrument.May determine that step instrument can meet the requirement of daily measurement by this error amount.
Use the present invention, a series of shoulder height can be prepared, such as 10 μm, 20 μm, 50 μm, 100 μm.Different height can also be designed for the specific requirement of step instrument.
Wherein, wet etching is a chemical reaction process purely, it is to utilize the chemical reaction between solution and pre-etachable material to remove the part sheltered for masked membrane material and reach to etch purpose, its shortcoming is: bore quarter serious, poor to the controlling of figure, the perpendicularity of the step i.e. obtained is poor, the step sample block directly using wet etching to prepare can not meet the requirement as standard substance, no longer carries out description of test at this.
The present invention is as a example by the print that nominal height is 50 μm, design two kinds of etch approach: DRIE etchings and DRIE etching+wet etching, wherein DRIE etching+wet etching is first to use DRIE etching, make etching depth close to step desired size namely the nominal height of standard sample that needs preparation, then use wet etching that the bottom surface of step is processed.The surface roughness of the print relatively completed.After having etched, the sample block roughness made is measured by the white light interferometer using Brooker company model to be GT-X8, and measurement result is as shown in table 1.
Table 1 be nominal height be the roughness measurement results of 50 μm prints
| Parameter | DRIE etches | DRIE etching+wet etching |
| Surface roughness Ra/nm | 11.4 | 6.2 |
Can be seen that the surface quality using DRIE etching+wet etching of the present invention to obtain is better than DRIE and etches the surface quality obtained from experimental result.
The stability of the sample block using DRIE etching+wet etching method to prepare 50 μm is monitored, in 12 months, step sample block has been carried out 12 stability assessments.As shown in figure 11, the result of appraisal show that the stability of sample block is (49.7468 ± 0.0166) μm to experimental result, and sample block does not occur significantly to change, and height value has preferable stability.
Claims (10)
1. the preparation method of nominal height 10 μm-100 μm standard step height sample block, it is characterised in that comprise the steps:
(1) use the silicon wafer (1) of twin polishing as backing material, clean, be dried；
(2) in silicon wafer (1) superficial growth oxide layer (2)；
(3) on oxide layer (2) surface resist coating (3), baking；
(4) by deep UV exposure, wherein mask plate is egative forme, and graphics field is transparent area；
(5) develop in aqueous slkali, remove the photoresist (3) of transparent area, then toast；
(6) use reactive ion etching machine to perform etching, the oxide layer (2) of the stepped area not having photoresist (3) to shelter is etched away；
(7) using deep reaction ion etching machine engraving erosion silicon wafer (1), perform etching the silicon wafer (1) of the stepped area not having photoresist (3) to shelter, etching depth is less than the nominal height of standard sample to be prepared；
(8) acetone soln is used to remove photoresist (3)；
(9) wet etching: the silicon wafer (1) of the stepped area not having oxide layer to shelter is proceeded etching, and etching depth reaches nominal height requirement, and etching terminates, cleaning silicon chip；
(10) on silicon wafer (1) surface splash-proofing sputtering metal protective layer (4), desired standard sample is prepared.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterized in that, in step (1), first use acid electronic cleaning agent, again with deionized water ultrasonic cleaning 10-20 minute, then use alkalescence electronic cleaning agent, then with deionized water ultrasonic cleaning 10-20 minute, dry 10-20 minute afterwards；Wherein the order of acid electronic cleaning agent and alkalescence electronic cleaning agent is interchangeable.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterised in that in step (2), uses thermal oxidation technology growth oxide layer (2), and the thickness of oxide layer (2) is 400 nm-500nm.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 3, it is characterized in that, in step (2), thermal oxidation technology is dry-oxygen oxidation+wet-oxygen oxidation+dry-oxygen oxidation, the method that wherein wet oxygen uses hydrogen-oxygen synthesis.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterised in that in step (3), thickness 3 μm-4 μm of photoresist (3), toast 5-15 minute at a temperature of 100-150 DEG C.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterized in that, in step (5), develop in NaOH solution, remove the photoresist of transparent area, then toast 5-15 minute at a temperature of 100-150 DEG C.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterised in that in step (6), etching gas is CHF3, and etch rate is 120-160nm/min.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterized in that, in step (7), etching depth is the nominal height μm that subtracts 5, etching gas is SF6 and C4F8, and etch rate is set as 4 μm/min-5 μm/min.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterized in that, in step (9), silicon wafer (1) is placed in the Tetramethylammonium hydroxide corrosive liquid that concentration is 47%, performing etching the silicon wafer (1) of the stepped area not having oxide layer (2) to shelter, etch rate is 1 μm/min；Etching terminates to use ultrasonic cleaning silicon chip.
The preparation method of a kind of nominal height 10 μm-100 μm standard step height sample block the most according to claim 1, it is characterised in that in step (10), coat of metal (4) is crome metal, and thickness is 80 nm-100nm.
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| CN109855572A (en) * | 2018-12-25 | 2019-06-07 | 中国电子科技集团公司第十三研究所 | For calibrating the line-spacing template and preparation method of optical profilometer roughness |
| CN111024016A (en) * | 2019-12-04 | 2020-04-17 | 中国电子科技集团公司第十三研究所 | Film thickness sample and preparation method of film thickness sample |
| CN111024017A (en) * | 2019-12-04 | 2020-04-17 | 中国电子科技集团公司第十三研究所 | Film thickness sample and preparation method of film thickness sample |
| CN112158794A (en) * | 2020-09-04 | 2021-01-01 | 杭州探真纳米科技有限公司 | Method for preparing atomic force microscope probe stepped substrate by adopting plasma etching |
| CN112158794B (en) * | 2020-09-04 | 2024-03-22 | 杭州探真纳米科技有限公司 | Method for preparing atomic force microscope probe stepped substrate by adopting plasma etching |
| CN112490115A (en) * | 2020-12-01 | 2021-03-12 | 苏州大学 | Transparent flexible monocrystalline silicon material and preparation method thereof |
| CN114543688A (en) * | 2022-01-17 | 2022-05-27 | 中国电子科技集团公司第十三研究所 | Step height standard sample block, preparation method and white light interferometer calibration method |
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