CN102520212A - Device for thinning multi-layer material and method for thinning to-be-detected sample - Google Patents
Device for thinning multi-layer material and method for thinning to-be-detected sample Download PDFInfo
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- CN102520212A CN102520212A CN2011104162162A CN201110416216A CN102520212A CN 102520212 A CN102520212 A CN 102520212A CN 2011104162162 A CN2011104162162 A CN 2011104162162A CN 201110416216 A CN201110416216 A CN 201110416216A CN 102520212 A CN102520212 A CN 102520212A
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Abstract
The invention provides a device for thinning a multi-layer material and a method for thinning a to-be-detected sample, belonging to the field of testing of semiconductors. The device comprises a reaction chamber, an atomic force microscope, an electron microscope and a sample table. The sample table, the atomic force microscope and the electron microscope are positioned in the reaction chamber. The method for thinning the to-be-detected sample comprises the following steps of: putting a sample in the reaction chamber; measuring first contact potential difference V1 of a first bared surface of the to-be-detected sample; moving away a conducting probe of the atomic force microscope; etching the first bared surface at the depth X to expose a second surface; measuring first contact potential difference V2 of a second bared surface of the to-be-detected sample; and comparing the V1 with the V2 to judge whether to etch continuously. The device and the method disclosed by the invention are used for solving the problem of being incapable of precisely dissecting in the prior art. The device and the method are capable of precisely dissecting hetero-junction devices and have important meanings on preparation and property research of semiconductor devices.
Description
Technical field
The present invention relates to the semiconducter device testing field, relate in particular to a kind of precise anatomical of heterojunction device.
Background technology
For for heterogeneous semiconductor junction devices such as efficient multi-node solar battery and LED, often comprise several and even dozens of heterojunction layer in its device architecture, realize device functions such as opto-electronic conversion through these heterogeneous interfaces.The character of each layer comprises that bed thickness, composition and doping content are all different, and has influence on the overall performance of device.For the character of each layer of test analysis, the good device of must will growing is usually dissected, and makes the layer exposed surface that will measure, successively measures its parameter, or processes cross-sectional slices, and methods such as employing transmission electron microscope are observed.
A kind of method of the heterogeneous lamination of precise anatomical is to adopt the focused-ion-beam lithography method, adopts the ion beam bombardment sample surfaces of certain accelerating potential and line, thereby produces the etching of sample surfaces.The bundle spot of FIB can be controlled in less than 10nm, thereby realizes accurate fixed point etching.In the process of ion beam etching; Usually need certain in site measurement means to know the degree of depth of etching and the lamination position that etches into; Usually the secondary electron imaging of adopting ion beam to produce at present, or adopt the pattern of scanning electron microscope home position observation etching position to judge speed of etching and position.But along with the application of nanostructureds such as quantum well in device, the bed thickness of these layers maybe be less than 10nm.The shortcoming that adopts method such as scanning electron microscope to observe is because the secondary electron imaging measurement obtains is two-dimensional image, can't accurately measure etching depth longitudinally, therefore for the thin layer of these nanostructureds, can't locate exactly.
Atomic force microscope is a kind of important characterization tool of nanoscale surface nature; It uses the tip curvature radius usually is the probe of tens nanometers; It is approached sample surfaces; Because the interaction between atoms power between probe and the sample makes probe overarm arm produce deformation, adopts the deformation of optical lever measuring probe, and utilize the feedback computing to make probe and sample room interaction force constant; Conducting probe just can obtain three-dimensional surface shape at surface scan then, and resolution can arrive nanoscale.On this basis as adopt the conduction conducting probe, can measure local force signals such as electric field force, magnetic field force, thus the local electric field of searching surface, magnetic field etc.
Summary of the invention
Technical matters to be solved by this invention is that a kind of attenuate device of multilayer material is provided.
In order to solve the problems of the technologies described above; The invention provides a kind of attenuate device of multilayer material; Comprise a reaction chamber, an atomic force microscope, a focused ion beam apparatus and a sample stage, said sample stage, atomic force microscope and focused-ion-beam lithography device are in the reaction chamber; Said sample stage is used to place testing sample; Said focused ion beam apparatus is used for the etching testing sample; Said atomic force microscope comprises conducting probe, is used for and testing sample contact and measure the contact potential difference between conducting probe and the testing sample.
Further comprise the one scan electron microscope, place in the said reaction chamber, be used for said testing sample and conducting probe imaging; Said atomic force microscope further comprises a micro-cantilever, links to each other with said conducting probe.
Further comprise a lock-in amplifier, place in the said reaction chamber, be used to survey the mechanical oscillation signal of conducting probe.
In order to solve the problems of the technologies described above, the present invention also provides a kind of method of utilizing like the attenuate device attenuate testing sample of above-mentioned multilayer material, comprises step:
1) with one have sandwich construction testing sample place in the reaction chamber;
2) utilize atomic force microscope to measure first exposed surface of testing sample and the first contact potential difference V1 of conducting probe;
3) remove the conducting probe of atomic force microscope;
4) utilize focused ion beam apparatus etching first exposed surface to the degree of depth X, expose second exposed surface;
5) utilize atomic force microscope to measure second exposed surface of testing sample and the second contact potential difference V2 of conducting probe;
6) relatively V1 and V2 are big or small, as | V1-V2|>Vm, then stop attenuate, otherwise repeating step 3 to 6, wherein Vm is a predefined threshold value.
The scope of said threshold value Vm is 10mV-1000mV; Etching depth X is not more than the smaller between said testing sample ground floor thickness and the second layer thickness.
In the said step 3, conducting probe is to remove through micro-cantilever, and the edge of removing back distance second exposed surface is greater than 1 μ m.
In the said step 2, when measuring the first contact potential difference V1, need to keep the constant distance of the conducting probe and first exposed surface, the scope of the distance of the said conducting probe and first exposed surface is 1nm-100nm; In the said step 5, when measuring the second contact potential difference V2, need to keep the constant distance of the conducting probe and second exposed surface, the scope of the distance of the said conducting probe and second exposed surface is 1nm-100nm.
Moving of said conducting probe need be guide with the image of electron microscope, comprises the positional information of conducting probe and testing sample in the said image.
Said step 2 further comprises the steps: under the contact mode of atomic force microscope, to measure the ground floor surface topography that obtains testing sample; Conducting probe is raised; Between the ground floor exposed surface of conducting probe and testing sample, apply an ac signal, drive the mechanical vibration of conducting probe generation and above-mentioned AC signal same frequency; Survey the conducting probe mechanical oscillation signal that above-mentioned AC signal frequency is caused, obtain the amplitude of vibration; Non-vanishing like the conducting probe vibration amplitude, then between the ground floor exposed surface of conducting probe and testing sample, apply a compensating direct current voltage, and adjust said compensating direct current voltage, be zero until the vibration amplitude of conducting probe; Making the conducting probe vibration amplitude is that zero compensating direct current magnitude of voltage is the first contact potential difference V1 between conducting probe and the testing sample ground floor exposed surface.
Said step 2 further comprises the steps: under the percussion mode of atomic force microscope, to measure the ground floor exposed surface pattern that obtains testing sample; The resonant frequency of the micro-cantilever under the said percussion mode is first AC signal, and said first AC signal causes that conducting probe produces one first mechanical vibration; Between the ground floor exposed surface of conducting probe and testing sample, apply one second AC signal, the electric field force that causes will drive one second mechanical vibration of the conducting probe generation and the second AC signal same frequency; Survey the frequency of first AC signal and the conducting probe mechanical oscillation signal that frequency caused of second AC signal, obtain the amplitude of first mechanical vibration and second mechanical vibration respectively; It is a constant that distance between adjusting conducting probe and testing sample makes the amplitude of the mechanical vibration of winning; Simultaneously between the ground floor exposed surface of conducting probe and testing sample, applying a compensating direct current voltage, and adjust said compensating direct current voltage, is zero until the amplitude of second mechanical vibration of conducting probe; The amplitude that makes second mechanical vibration of conducting probe is that zero compensating direct current magnitude of voltage is the first contact potential difference V1 between conducting probe and the testing sample ground floor exposed surface.
Also comprise step before the said step 1:, judge that whether ground floor thickness is greater than second layer thickness according to the thickness of given said ground floor and the thickness of the second layer; If ground floor thickness, then utilizes exposed surface to the degree of depth Y of focused ion beam apparatus etching testing sample greater than second layer thickness, the exposed surface that etching is exposed is as first exposed surface; Otherwise with the exposed surface of testing sample as first exposed surface.
Said etching depth Y is the thickness size that is not more than the greater between the thickness size of thickness size and the second layer of said ground floor.
The invention has the advantages that, utilize the conducting probe in site measurement surface potential function of atomic force microscope, come assisted focused ion beam to know the degree of depth and the number of plies of etching.Each layer in the multilayer material is because composition and dopant species different; Make its surface potential that bigger difference arranged; And measure the surperficial contact potential difference between conducting probe and the testing sample based on conducting probe; Its measuring accuracy can be less than 10mV, can solve the original position etching control problem of multilayer material attenuate effectively, and is significant to the preparation and the property research of semiconductor devices.
Description of drawings
Fig. 1 is attenuate device embodiment one synoptic diagram of multilayer material provided by the invention;
Fig. 2 is method embodiment two flow chart of steps of attenuate testing sample provided by the invention;
Fig. 3 A～3G is the method embodiment two measuring process figure of attenuate testing sample provided by the invention;
Fig. 4 is the preferred implementation flow chart of steps of method embodiment two steps 303 of attenuate testing sample provided by the invention;
Fig. 5 is a testing sample structural representation among the method embodiment three of attenuate testing sample provided by the invention.
Embodiment
Elaborate below in conjunction with the embodiment of accompanying drawing to the method for the attenuate device of multilayer material provided by the invention and attenuate testing sample.
Embodiment one
Shown in Figure 1 is the attenuate device of a kind of multilayer material provided by the invention; Comprise a reaction chamber 110, an atomic force microscope, a focused ion beam apparatus 103; One electron microscope 102 and a sample stage 100, and sample stage 100, focused ion beam apparatus 103, atomic force microscope and electron microscope 102 are in the reaction chamber 110; Sample stage 100 is used to place testing sample; Atomic force microscope is used to measure testing sample surface contact potential difference, comprises conducting probe 105, micro-cantilever 104 and control device 106; Focused ion beam apparatus 103 is used for the etching testing sample; Conducting probe 105 is used for and testing sample contacts and measure the contact potential difference between conducting probe and the testing sample; Micro-cantilever 104 is used for moving conducting probe 105; Electron microscope 102 is used for the testing sample surface location is formed images.
Embodiment two
Shown in Figure 2 is method embodiment two flow chart of steps of attenuate testing sample provided by the invention, comprising: step 301, with one have sandwich construction testing sample place in the reaction chamber; Step 302 moves to the testing sample top with the atomic force microscope conducting probe; Step 303 utilizes atomic force microscope to measure first exposed surface of testing sample and the first contact potential difference V1 of conducting probe; Step 304 is removed the conducting probe of atomic force microscope; Step 305 is utilized focused ion beam apparatus etching first exposed surface to the degree of depth X, exposes second exposed surface; Step 306 utilizes atomic force microscope to measure the second contact potential difference V2 of second exposed surface and conducting probe; Step 307, relatively V1 and V2 are big or small, as | V1-V2|>Vm, then stop attenuate, otherwise repeating step 303 to 306, wherein Vm is a predefined threshold value.
Fig. 3 A is depicted as method embodiment two steps 301 of attenuate testing sample provided by the invention, and testing sample 402 is placed on the sample stage 401, and wherein testing sample 402 comprises ground floor 402a, second layer 402b and the 3rd layer of 402c;
Fig. 3 B is depicted as method embodiment two steps 302 of attenuate testing sample provided by the invention; The etch areas of the ground floor 402a exposed surface appointment through 404 pairs of testing samples 402 of electron microscope and the imaging of conducting probe 403 positions of atomic force microscope; Move conducting probe 403 through micro-cantilever 405 simultaneously; Under the guide of the image that electron microscope 404 records, conducting probe 403 is moved to the ion beam etching machining area top of ground floor 402a exposed surface;
Fig. 3 C is depicted as method embodiment two steps 303 of attenuate testing sample provided by the invention; The first contact potential difference V1 between the ground floor 402a exposed surface of measurement conducting probe 403 and testing sample 402, and the spacing range of the conducting probe and first exposed surface is 1nm-100nm.
Fig. 3 D is depicted as method embodiment two steps 304 of attenuate testing sample provided by the invention; Through 404 pairs of etch areas of electron microscope and the imaging of conducting probe 403 positions; Move Edge Distance that conducting probe 403 leaves etch areas greater than 1 μ m through micro-cantilever 405, prevent FIB damage conducting probe 403.
Fig. 3 E is depicted as method embodiment two steps 305 of attenuate testing sample provided by the invention, opens focused ion beam apparatus 406, and the size that provides during according to device fabrication is set etching depth X.Etch areas to the ground floor 402a exposed surface of testing sample 402 is carried out etching, and etching operation is closed focused ion beam apparatus 406 after accomplishing.The size of etching depth X should be for being not more than the smaller's between said testing sample 402 ground floor 402a thickness and the second layer 402b thickness thickness size.Usually the thickness of each layer growth has discreet value in the device, can correlation parameter be provided by the technician of growth of device.The thickness size of selected said ground floor 402a and the thickness size of second layer 402b compare, and the smaller among both is as the maximal value of etching depth X.Fig. 3 F is depicted as method embodiment two steps 306 of attenuate testing sample provided by the invention, repeating step 303, the contact potential difference V2 between the exposed surface of measurement conducting probe 403 and etch areas.
Fig. 3 G is depicted as method embodiment two steps 307 of attenuate testing sample provided by the invention; Relatively the size of contact potential difference V2 and contact potential difference V1, is just thought to have etched into second layer 402b greater than Vm like both; Can stop etching; Otherwise think that then the exposed surface of etch areas still belongs to ground floor 402a, then need continue execution in step 304～step 307, wherein Vm is a predefined threshold value.The scope of threshold value Vm is 10mV ~ 1000mV.
Continue accurate etching second layer 402b like needs, can just repeat above-mentioned steps 301～307.
As a kind of optional embodiment, also comprise step before the said step 1: the thickness of each layer growth has discreet value in the device usually, can correlation parameter be provided by the technician of growth of device.According to the thickness of given said ground floor 402a and the thickness of second layer 402b, judge that whether ground floor 402a thickness is greater than second layer 402b thickness; If ground floor 402a thickness, then utilizes exposed surface to the degree of depth Y of focused ion beam apparatus etching testing sample 402 greater than second layer 402b thickness, the exposed surface that etching is exposed is as first exposed surface; Otherwise with the exposed surface of testing sample 402 as first exposed surface.
Said etching depth Y is the thickness size that is not more than the greater between the thickness size of thickness size and second layer 402b of said ground floor 402a.
Shown in Figure 4 is the preferred implementation flow chart of steps of method embodiment two steps 303 of attenuate testing sample provided by the invention.As one preferred embodiment, step 303 may further include following steps:
The above is merely the preferred implementation of embodiment two steps 303; This step can also adopt other embodiments to measure; A kind of enforcement wherein comprises the steps: that the ground floor 402a exposed surface of conducting probe 403 and testing sample 402 periodically contacts; The percussion mode that adopts atomic force microscope is down through measuring the ground floor 402a exposed surface pattern that obtains testing sample 402; The resonant frequency of the micro-cantilever 405 under the said percussion mode is first AC signal, and said first AC signal causes that conducting probe 403 produces one first mechanical vibration; Between the ground floor 402a of conducting probe 403 and testing sample 402 exposed surface, apply one second AC signal, the electric field force that causes will drive one second mechanical vibration of conducting probe 403 generations and the second AC signal same frequency; Adopt lock-in amplifier to survey the frequency of first AC signal and the conducting probe that frequency caused 403 mechanical oscillation signals of second AC signal, obtain the amplitude of first mechanical vibration and second mechanical vibration respectively; It is a constant that the distance that adjusting conducting probe 403 and testing sample are 402 makes the amplitude of the mechanical vibration of winning; Simultaneously between the ground floor 402a of conducting probe 403 and testing sample 402 exposed surface, applying a compensating direct current voltage, and adjust said compensating direct current voltage, is zero until the amplitude of second mechanical vibration of conducting probe 403; The amplitude that makes second mechanical vibration of conducting probe 403 is that zero compensating direct current magnitude of voltage is the first contact potential difference V1 between conducting probe 403 and the testing sample 402 ground floor 402a exposed surfaces.
Embodiment three
Shown in Figure 5 is testing sample structural representation among the method embodiment three of attenuate testing sample provided by the invention.Testing sample 206 has the heterogeneous multi-layer junction structure, comprises p
+GaAs layer 205, p
+AlGaAs layer 204, p
+GaAs layer 203, InGaAs layer 202, n
-GaAs layer 201, n
+GaAs layer 200 and n
-GaAs substrate layer 210.And the bed thickness of above-mentioned layer structure is respectively 0.5 μ m, 0.03 μ m, 0.5 μ m, 0.02 μ m, 2 μ m, 0.5 μ m.
The method of attenuate testing sample 206 comprises: testing sample 206 is placed in the reaction chamber; Through etch areas and the conducting probe position imaging of electron microscope to p+GaAs layer 205 appointment of sample; Move conducting probe through micro-cantilever simultaneously; Under the guide of electron microscope image, the atomic force microscope conducting probe is moved to ion beam etching machining area top; Measure the first contact potential difference V1 between conducting probe and the testing sample; To etch areas and the imaging of conducting probe position, the Edge Distance that leaves etch areas through the micro-cantilever traveling probe prevents FIB damage conducting probe greater than 1 μ m through electron microscope; Open focused ion beam apparatus, the ion beam accelerating potential is made as 25KV and line is made as 10pA, and the size that provides during again according to device fabrication is set etching depth X, because p
+The bed thickness of GaAs layer 205 is 0.5 μ m, and therefore setting etching time is 480 seconds, and etching depth X gets 0.48 μ m micron, to p
+The etch areas of GaAs layer 205 is carried out etching, the about 1nm/s of etch rate, and etching operation is closed focused ion beam apparatus after accomplishing; Contact potential difference V2 between the exposed surface of measurement conducting probe and etch areas; Relatively the size of contact potential difference V2 and contact potential difference V1, is just thought to have etched into p greater than 20mV like both
+ AlGaAs layer 204 can stop etching, otherwise thinks that then the exposed surface of etch areas still belongs to p
+GaAs layer 205 then need continue to carry out etching, but should adjust, and should reduce I.B.M. time and etching depth, as etching time being set at 10s, each about 10nm of etching depth.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (12)
1. the attenuate device of a multilayer material is characterized in that, comprises a reaction chamber, an atomic force microscope, a focused ion beam apparatus and a sample stage, and said sample stage, atomic force microscope and focused-ion-beam lithography device are in the reaction chamber; Said sample stage is used to place testing sample; Said focused ion beam apparatus is used for the etching testing sample; Said atomic force microscope comprises conducting probe, is used for and testing sample contact and measure the contact potential difference between conducting probe and the testing sample.
2. the attenuate device of multilayer material according to claim 1 is characterized in that, further comprises the one scan electron microscope, places in the said reaction chamber, is used for said testing sample and conducting probe imaging; Said atomic force microscope further comprises a micro-cantilever, links to each other with said conducting probe.
3. the attenuate device of multilayer material according to claim 1 is characterized in that, further comprises a lock-in amplifier, places in the said reaction chamber, is used to survey the mechanical oscillation signal of conducting probe.
4. a method of utilizing the attenuate device attenuate testing sample of multilayer material as claimed in claim 1 is characterized in that, comprises step:
1) with one have sandwich construction testing sample place in the reaction chamber;
2) utilize atomic force microscope to measure first exposed surface of testing sample and the first contact potential difference V1 of conducting probe;
3) remove the conducting probe of atomic force microscope;
4) utilize focused ion beam apparatus etching first exposed surface to the degree of depth X, expose second exposed surface;
5) utilize atomic force microscope to measure second exposed surface of testing sample and the second contact potential difference V2 of conducting probe;
6) relatively V1 and V2 are big or small, as | V1-V2|>Vm, then stop attenuate, otherwise repeating step 3 to 6, wherein Vm is a predefined threshold value.
5. the method for attenuate testing sample according to claim 4 is characterized in that, the scope of said threshold value Vm is 10mV-1000mV; Etching depth X is not more than the smaller between said testing sample ground floor thickness and the second layer thickness.
6. the method for attenuate testing sample according to claim 4 is characterized in that, in the said step 3, conducting probe is to remove through micro-cantilever, and the edge of removing back distance second exposed surface is greater than 1 μ m.
7. the method for attenuate testing sample according to claim 4; It is characterized in that; In the said step 2; When measuring the first contact potential difference V1, need to keep the constant distance of the conducting probe and first exposed surface, the scope of the distance of the said conducting probe and first exposed surface is 1nm-100nm; In the said step 5, when measuring the second contact potential difference V2, need to keep the constant distance of the conducting probe and second exposed surface, the scope of the distance of the said conducting probe and second exposed surface is 1nm-100nm.
8. the method for attenuate testing sample according to claim 4 is characterized in that, moving of said conducting probe need be guide with the image of electron microscope, comprises the positional information of conducting probe and testing sample in the said image.
9. the method for attenuate testing sample according to claim 4 is characterized in that, said step 2 further comprises the steps: under the contact mode of atomic force microscope, to measure the ground floor surface topography that obtains testing sample; Conducting probe is raised; Between the ground floor exposed surface of conducting probe and testing sample, apply an ac signal, drive the mechanical vibration of conducting probe generation and above-mentioned AC signal same frequency; Survey the conducting probe mechanical oscillation signal that above-mentioned AC signal frequency is caused, obtain the amplitude of vibration; Non-vanishing like the conducting probe vibration amplitude, then between the ground floor exposed surface of conducting probe and testing sample, apply a compensating direct current voltage, and adjust said compensating direct current voltage, be zero until the vibration amplitude of conducting probe; Making the conducting probe vibration amplitude is that zero compensating direct current magnitude of voltage is the first contact potential difference V1 between conducting probe and the testing sample ground floor exposed surface.
10. the method for attenuate testing sample according to claim 4; It is characterized in that; Said step 2 further comprises the steps: under the percussion mode of atomic force microscope, to measure the ground floor exposed surface pattern that obtains testing sample; The resonant frequency of the micro-cantilever under the said percussion mode is first AC signal, and said first AC signal causes that conducting probe produces one first mechanical vibration; Between the ground floor exposed surface of conducting probe and testing sample, apply one second AC signal, the electric field force that causes will drive one second mechanical vibration of the conducting probe generation and the second AC signal same frequency; Survey the frequency of first AC signal and the conducting probe mechanical oscillation signal that frequency caused of second AC signal, obtain the amplitude of first mechanical vibration and second mechanical vibration respectively; It is a constant that distance between adjusting conducting probe and testing sample makes the amplitude of the mechanical vibration of winning; Simultaneously between the ground floor exposed surface of conducting probe and testing sample, applying a compensating direct current voltage, and adjust said compensating direct current voltage, is zero until the amplitude of second mechanical vibration of conducting probe; The amplitude that makes second mechanical vibration of conducting probe is that zero compensating direct current magnitude of voltage is the first contact potential difference V1 between conducting probe and the testing sample ground floor exposed surface.
11. the method for attenuate testing sample according to claim 4 is characterized in that, also comprises step before the said step 1: according to the thickness of given said ground floor and the thickness of the second layer, judge that whether ground floor thickness is greater than second layer thickness; If ground floor thickness, then utilizes exposed surface to the degree of depth Y of focused ion beam apparatus etching testing sample greater than second layer thickness, the exposed surface that etching is exposed is as first exposed surface; Otherwise with the exposed surface of testing sample as first exposed surface.
12. the method for attenuate testing sample according to claim 11 is characterized in that, said etching depth Y is the thickness size that is not more than the greater between the thickness size of thickness size and the second layer of said ground floor.
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| CN102520212B (en) | 2013-10-30 |
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