CN110165056A - A kind of CTM memory and preparation method thereof - Google Patents
A kind of CTM memory and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000009825 accumulation Methods 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000002105 nanoparticle Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 14
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 10
- -1 siloxanes Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 3
- 238000003491 array Methods 0.000 claims description 3
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims description 2
- 239000011147 inorganic material Substances 0.000 claims description 2
- 239000011368 organic material Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 235000013339 cereals Nutrition 0.000 claims 1
- 230000003111 delayed effect Effects 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007850 degeneration Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 21
- 239000010408 film Substances 0.000 description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RWHRFHQRVDUPIK-UHFFFAOYSA-N 50867-57-7 Chemical compound CC(=C)C(O)=O.CC(=C)C(O)=O RWHRFHQRVDUPIK-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
- H10K10/20—Organic diodes
- H10K10/29—Diodes comprising organic-inorganic heterojunctions
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
- H10K10/80—Constructional details
- H10K10/82—Electrodes
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/40—Organosilicon compounds, e.g. TIPS pentacene
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
Abstract
The invention belongs to technical field of electronic devices, disclose the organic-inorganic mixing CTM memory and preparation method thereof of zirconium oxide and zirconium silicate nano particle, CTM memory includes the lower electrode being stacked from the bottom to top, substrate, accumulation layer and upper electrode layer；The accumulation layer is the organic-inorganic hybrid layer of material containing zirconium oxide and zirconium silicate nano particle.The present invention prepares accumulation layer using solwution method, realizes that the preparation of low cost CTM, equipment and raw material investment are less, it can be achieved that large-scale industrial application.In addition, accumulation layer that the preparation method that the present invention uses is prepared while having tunnel layer, the effect of accumulation layer and barrier layer reduces technology difficulty, reduces the degeneration of device performance caused by complicated technology.
Description
Technical field
The present invention relates to microelectronics technology, specifically a kind of organic nothing based on zirconium oxide and zirconium silicate nano particle
The CTM and preparation method thereof of machine mixing material.
Background technique
Memory is many kinds of, can be divided into magnetic surface storage and semiconductor memory according to storage material, and semiconductor
Memory can be divided into volatile memory and nonvolatile memory according to whether data preservation relies on external power supply again.It is volatile
Property memory can lose the data of all storages, such as dynamic memory (DRAM), static memory (SRAM) after a loss of power.Phase
Instead, even if nonvolatile memory in the event of a power failure, is also able to maintain the data of storage, such as flash memory (Flash), electric charge capture
Type memory (CTM) etc..CTM has its low-power consumption, and fatigue properties are good, and the strong feature of data holding ability, is used at present
One of mainstream nonvolatile memory.Charge tunnelling disengaging accumulation layer is controlled by applying different voltage in accumulation layer,
To realize the write-in of data, erasing and storage.The existing research for CTM be concentrated mainly on storage material screening and it is excellent
Change, storage density is promoted, device architecture optimization and optimum preparation condition.Wherein, grinding for device architecture and preparation process
Study carefully most important.Traditional CTM structure is " lower electrode/substrate/tunnel layer/accumulation layer/barrier layer/top electrode ", film layer one
As by atomic layer deposition (ALD), the methods of sputtering and chemical vapor deposition preparation, but the above method is limited to equipment, production
Cost is excessively high, is unable to satisfy the industrial production demand of low cost.In addition, traditional multilayered structure is in complicated preparation process
The degeneration that will lead to device performance is unfavorable for improving production efficiency.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of organic-inorganic based on zirconium oxide and zirconium silicate nano particle
CTM of mixing material and preparation method thereof can be reduced caused device performance degeneration in complicated preparation process, can satisfy simultaneously
The industrial requirement of low cost production.
The present invention is achieved by the following technical solutions:
The first aspect of the present invention provides a kind of organic-inorganic mixing material based on zirconium oxide and zirconium silicate nano particle
CTM memory, including the lower electrode layer being stacked from the bottom to top, substrate, accumulation layer and upper electrode layer；The accumulation layer is
The film layer of organic and inorganic mixing material.
Preferably, the substrate is silicon membrane layer, with a thickness of 280-320nm.
Preferably, the upper electrode layer includes top electrode of several arrays in accumulation layer.
Described to power on extremely cylinda gold category aluminum film layer, with a thickness of 800-900nm, area is 1.4-1.8 × 10-9cm2。
Preferably, the organic material is siloxanes, and inorganic material is zirconium oxide and zirconium silicate particles.
Preferably, zirconium oxide and zirconium silicate are nano particle, nano-particle diameter 20-25nm, film thickness 500-
600nm。
Second aspect of the present invention provides the process of preparing of above-mentioned CTM memory, includes the steps that preparing accumulation layer, tool
Body includes the following:
(1) accumulation layer precursor solution is prepared
Meanwhile zirconium-n-propylate, methacrylic acid and normal propyl alcohol solution being mixed and stirred for obtaining according to molar ratio 1:1:1
Solution A；Dilute hydrochloric acid is added in 3- (methacryloxypropyl) propyl trimethoxy silicane solution and stirs to get solution B；It will match
The A liquid set is added in B liquid, and the two volume ratio is 0.5-2, and it is molten to be stirring evenly and then adding into 1- hydroxycyclohexyl phenyl ketone
Liquid；It is eventually adding normal propyl alcohol and obtains precursor solution；
(2) accumulation layer is prepared
Substrate is immersed in precursor solution above-mentioned and is slowly lifted, then substrate is placed on hot plate preannealing until
Then solution freezing film irradiates the film to be formed with UV lamp, finally substrate is placed on hot plate and is annealed, and is made and deposits in substrate
Reservoir.
Preferably, in step (2), then by substrate as progress preannealing on hot plate to solution freezing film, preannealing
Temperature is 100-120 DEG C, time 25-35min.
Preferably, in step (2), in step (2), the film that UV lamp forms preannealing is irradiated, and UV lamp power is
10-20mW, UV lamp irradiation time are 5-8min.
Preferably, in step (2), annealing temperature is 150-250 DEG C, and the time is 2-5 hours, and accumulation layer is made.
Preferably, the substrate first passes through hydrofluoric acid aqueous solution cleaning.Preferably, electrode material is metallic aluminium.
Preferably, after step (2), liquid electrode material is coated in by accumulation layer and base by silk screen print method respectively
On bottom, top electrode and lower electrode are formed, top electrode and lower thickness of electrode are 800-900nm.
Technical effect
Compared with prior art, the present invention has the following technical effect that
1) accumulation layer of CTM memory of the present invention has equally distributed zirconium oxide and zirconium silicate nano particle, so that packet
It wraps up in nano particle siloxanes while having the function of tunnel layer and barrier layer, answering for film layer is repeatedly prepared compared to traditional handicraft
Miscellaneous process has reduced caused device degradation during preparation process tunnel layer and barrier layer.
2) present invention prepares accumulation layer using pure solwution method, simple to operate, realizes the CTM preparation of low cost, if
The less preparation that can be used for large area CTM device is invested for and with raw material, realizes large-scale industrial application.
3) present invention uses elemental metals or elemental metals compound-material as top electrode, instead of traditional oxide
Material top electrode further reduces costs and optimizes preparation process.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of CTM device prepared by embodiment 1；
Fig. 2 is memory window characteristic variations figure of the embodiment 1 within the scope of 170-200 DEG C；Wherein, top electrode 100, storage
Layer 200, zirconium oxide and zirconium silicate nano particle 201, substrate 300, lower electrode layer 400；
Fig. 3 is the memory window test result of CTM device prepared by embodiment 1.
Specific embodiment
The specific embodiment of the invention is described below in conjunction with attached drawing.
Embodiment 1
As shown in Figure 1, this example is related to a kind of organic-inorganic mixing material based on zirconium oxide and zirconium silicate nano particle
CTM, including the lower electrode 400 being stacked from the bottom to top, substrate 300, accumulation layer 200 and upper electrode layer 100；
The upper electrode layer includes cylindricality top electrode 100 of several arrays in accumulation layer 200, with a thickness of 800-900nm,
Area is 1.4-1.8 × 10-9cm2, it is preferred that with a thickness of 830nm, area is 1.6 × 10-9cm2；
The accumulation layer 200 is the organic-inorganic hybrid layer of material containing zirconium oxide and zirconium silicate nano particle 201, material
For siloxanes, with a thickness of 500-600nm, nano-particle diameter 20-25nm, it is preferred that with a thickness of 560nm, radius 22nm；
The substrate 300 is silicon wafer, with a thickness of 280-320 μm, it is preferred that with a thickness of 300 μm；
The lower electrode layer 400 is metal aluminium film, with a thickness of 500-600nm, it is preferred that with a thickness of 530nm.
This example is related to the process of preparing of above-mentioned CTM, comprising:
A) substrate 300 is cleaned；
Substrate 300 is completely immersed in and is held in the aqueous solution containing 4% hydrofluoric acid (HfO2), impregnate 60 seconds after, spend from
Sub- water rinses substrate 300 and removes remaining impurity and with being dried with nitrogen.
B) precursor solution is prepared；
The 3- (methacryloxypropyl) third that the concentration of 10-20mL is 2M is added in the dilute hydrochloric acid (HCl) that 5mL concentration is 0.2M
In base trimethoxy silane solution (3-Methacryloxypropyltrimethoxysilane) and stir 30 minutes；Meanwhile
By zirconium-n-propylate (Zr (OPri)4), methacrylic acid (methacrylic acid) and normal propyl alcohol (1-propanol) solution are pressed
It is mixed and stirred for 30 minutes according to molar ratio 1:1:1.By configured zirconium-n-propylate (Zr (OPri) after stirring4) solution adds
Enter configured 3- (methacryloxypropyl) propyl trimethoxy silicane solution (3-Methacryloxypropyltrimethox
Ysilane) in solution, the two ratio is 0.5-2, and the deionized water of 5-10mL is then added and stirs 24 hours.Stirring finishes
1- hydroxycyclohexyl phenyl ketone solution (the 1-hydroxycyclohexyl phenyl that 3-6mL concentration is 0.5M is added afterwards
ketone)；It is eventually adding the normal propyl alcohol solution (1-propanol) of 2-5mL and stirs 30 minutes obtained precursor solutions.
C) accumulation layer 200 is prepared；
Substrate 300 is fully immersed in configured precursor solution and is lifted, pull rate is no more than
100mm/min, lifting time are 25-35s.After lifting, substrate 300 is solidified as preannealing to solution is carried out on hot plate
Film forming, Pre-annealing Temperature are 100-120 DEG C, time 25-35min.After preannealing, preannealing is formed with UV lamp thin
Film is irradiated, and UV lamp power is 10-20mW, and UV lamp irradiation time is 5-8min.After irradiation, by substrate 300 as heat
It anneals on plate, annealing temperature is 150-250 DEG C, and the time is 2-5 hours, and accumulation layer 200 is made.
D) top electrode 100 and lower electrode layer 400 are prepared；
Liquid upper electrode material is coated in accumulation layer and substrate by silk screen print method, forms 100 He of top electrode
Lower electrode 400, material are metallic aluminium, and for top electrode with a thickness of 800-900nm, area is 1.4-1.8 × 10-9cm2。
It is illustrated in figure 2 the SEM picture of this example accumulation layer, as can be seen from the figure zirconium oxide and zirconium silicate nano particle
It is evenly distributed in siloxanes, average diameter 20-25nm.
It is illustrated in figure 3 the memory window test result of this example CTM device, alive is gradually increased (± 5 with applying
To ± 10V), memory window has apparent increase, and maximum can embody good storage characteristics to 11V.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel only illustrate the present invention it should be appreciated that the present invention is not limited by examples detailed above described in examples detailed above and specification
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its is equal
Object defines.
Claims (10)
1. a kind of CTM memory, which is characterized in that including the lower electrode layer being stacked from the bottom to top, substrate, accumulation layer and upper
Electrode layer；The accumulation layer is the film layer of machine, inorganic hybrid materials.
2. CTM memory according to claim 1, which is characterized in that the organic material is siloxanes, and inorganic material is
Zirconium oxide and zirconium silicate particles.
3. CTM memory according to claim 2, which is characterized in that the zirconium oxide and zirconium silicate are nano particle, are received
Rice grain diameter is 20-25nm.
4. CTM memory according to claim 1, which is characterized in that the upper electrode layer includes that several arrays are storing
Top electrode on layer.
5. CTM memory according to claim 1, which is characterized in that described to power on extremely cylinda gold category aluminum film layer.
6. the method for preparing CTM memory as described in any one in claim 1-5 includes the steps that preparing accumulation layer, specifically
Include the following:
(1) accumulation layer precursor solution is prepared
Meanwhile zirconium-n-propylate, methacrylic acid and normal propyl alcohol solution being mixed and stirred for obtaining solution according to molar ratio 1:1:1
A；Dilute hydrochloric acid is added in 3- (methacryloxypropyl) propyl trimethoxy silicane solution and stirs to get solution B；It will configure
A liquid be added B liquid in, the two volume ratio be 0.5-2, be stirring evenly and then adding into 1- hydroxycyclohexyl phenyl ketone solution；Most
Normal propyl alcohol is added afterwards and obtains precursor solution；
(2) accumulation layer is prepared
Substrate is immersed in precursor solution above-mentioned and is slowly lifted, then substrate is placed in preannealing on hot plate until solution
Then freezing film irradiates the film to be formed with UV lamp, finally substrate is placed on hot plate and is annealed, and storage is made in substrate
Layer.
7. according to the method described in claim 6, it is characterized in that, substrate being immersed in precursor solution and is delayed in step (2)
Slow lifting, pull rate are no more than 100mm/min, and the lifting time is 25-35s.
8. according to the method described in claim 6, it is characterized in that, then substrate is carried out in advance as on hot plate in step (2)
It is annealed to solution freezing film, Pre-annealing Temperature is 100-120 DEG C, time 25-35min.
9. according to the method described in claim 6, it is characterized in that, in step (2), UV lamp forms preannealing in step (2)
Film be irradiated, UV lamp power be 10-20mW, UV lamp irradiation time be 5-8min.
10. CTM memory according to claim 6, which is characterized in that in step (2), annealing temperature is 150-250 DEG C,
Time is 2-5 hours, and accumulation layer is made.
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| US20060141703A1 (en) * | 2004-12-24 | 2006-06-29 | Samsung Electronics Co., Ltd. | Method of manufacturing nonvolatile organic memory device and nonvolatile organic memory device manufactured by the same |
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