CN105887038A - Method for etching boron-doped diamonds - Google Patents
Method for etching boron-doped diamonds Download PDFInfo
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- CN105887038A CN105887038A CN201610237371.0A CN201610237371A CN105887038A CN 105887038 A CN105887038 A CN 105887038A CN 201610237371 A CN201610237371 A CN 201610237371A CN 105887038 A CN105887038 A CN 105887038A
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- boron
- etching
- doped diamond
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- sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5826—Treatment with charged particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5873—Removal of material
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for etching boron-doped diamonds, and relates to the novel electronic material technology. An ultrahigh-vacuum magnetron sputtering machine and direct-current arc plasma jetting CVD equipment are adopted for preparing the diamonds, firstly sputtering of nickel nano-particles is carried out through the magnetron sputtering method, then plasma etching of the boron-doped diamonds is carried out with the nickel nano-particles as catalysts, and finally target products are prepared. The method has the advantages that the porous diamonds are easily machined and formed and play a key role in actual application of the novel electronic function material; the technology is simple, implementation is easy, the use rate of targets is high, and the production cost is low. Thus, the method is suitable for wide application and popularization.
Description
Technical field
The present invention relates to novel electron material technology technology, the method for a kind of boron-doped diamond etching.
Background technology
Diamond has many remarkable physicochemical properties, such as light weight, intensity corruption high, wear-resistant, anti-
Erosion, heat conductivity, good insulating, push it against actual application always people's emphasis and the direction of effort.Mesh
Before the application that has been carried out have the superhard coating of cutting element, diaphragm of loudspeaker coating, laser instrument and collection
Become circuit heat sink, X-ray window material and mask plate backing material, optical element coating etc..
The diamond film MEMS succeeded in developing is the rarest, the most several example special sensors,
In addition, only some simple micro structures, such as overarm arm etc., occur this situation main cause it
One is exactly that diamond is difficult to processed.
Diamond micropowder processes main selective growth and etching two big classes, and etching mainly has wet method and dry method
Two big classes.Selective growth is first to be deposited on substrate by exotic material, and recycling photoetching technique etches
Required figure, then carries out the growth of diamond film, is finally removed by mask；Etching method mainly by
Dry etching technology directly carves required figure on diamond film.Spy due to diamond film growth condition
Different property, the selectivity of growth district is to be determined do not have marginal mask by the nucleus Forming ability of initial surface
Constraint, along with the increase of film thickness, its lateral growth can hardly be avoided, therefore significantly reduce this technique
The dimensional accuracy of machine-shaping micro structure, the most also thick film grows the sparse crystalline substance in issuable disactivation region
The structure cohesion that core continued propagation is caused, so the effect of selective growth not fully up to expectations.Therefore,
Mainly having laser ablation micro Process and reactive ion etching, laser ablation micro Process is with general dry etching not
With, many employing laser beam flying modes are carried out, and in addition to requiring further improvement hachure working ability, add
Work efficiency rate is the most in urgent need to be improved.By comparison, reactive ion etching has more advantage, in contemporary electronic work
In industry, it, as a kind of traditional technology, is usually used in the etching of diamond.
Summary of the invention
It is an object of the invention to for above-mentioned technical Analysis, it is provided that the method for the etching of a kind of boron-doped diamond,
I.e. sputter nano nickel particles initially with magnetron sputtering method, carving as catalyst plasma using nano nickel particles
Erosion boron-doped diamond, the operation of this lithographic method is fairly simple, and etching effect is more preferably.
Technical scheme:
The method of a kind of boron-doped diamond etching, step is as follows
1) negative electrode at magnetron sputtering coater installs nickel target, anode fixed diamond sheet；
2) open target magnetic control sputtering equipment, successively start one-level mechanical pump and secondary molecules pumping vacuum；
3) it is passed through argon to vacuum chamber；
4) open shielding power supply, nickel target apply electric current and voltage, carries out pre-sputtering, wait sputtering current and
Voltage stabilization；Opening the baffle plate in substrate frame and start plated film, in coating process, substrate position is fixed；
5) after plated film terminates, close the baffle plate in substrate frame, be then shut off shielding power supply, stop being passed through sputtering
Gases argon, fully opens gate valve, continues evacuation, is then shut off vacuum system, after system cools down
It is filled with air to vacuum chamber, when the air pressure of vacuum chamber is identical with external atmosphere pressure, opens vacuum chamber, open sample
Product take out the boron-doped diamond sheet of nickel plating；
6) sample stage that the boron-doped diamond sheet of nickel plating is placed in DC arc plasma jet CVD equipment props up
On frame；
7) open power distribution cabinet, open electrical control cabinet, open water-cooling system and mechanical pump evacuation, evacuation
After end, it is passed through hydrogen and argon, waits that chamber pressure, pump pressure are gone up；
8) control switch in magnetic field is opened, annealing, by controlling sample stage height, controls temperature；
9) close electrical control cabinet and power distribution cabinet after annealing terminates, after cooling down etc. deposition table, take out the mesh prepared
Mark product.
Step 2) in until the back end vacuum of sputtering chamber is 1 × 10-4Pa。
Step 4) in the pre-sputtering time be 20 minutes；The plated film time is 1 minute.
Step 7) in, when chamber pressure, pump pressure are all stablized at below 3000Pa, open the lobe pump degree of depth and take out very
Sky, during until chamber pressure and pump pressure are below 0.1Pa, is passed through hydrogen or argon.
Step 7) in, chamber pushes back and rises to 3000Pa, and pump pressure is gone up to 13000Pa.
Step 8) in, magnetic field controls switch and opens, and tune voltage is 6.0V, and arc power controls igniting and opens,
Anneal 6 minutes.
The purity of described nickel target is 99.99%, and the thickness of target is 5mm, a diameter of 60mm；
Described argon, the purity of hydrogen is 99.999%, in superhigh vacuum magnetron sputtering film-plating machine, argon
Flow be 15sccm；In DC arc plasma jet CVD equipment, the flow of hydrogen and argon is
1.5L/min；
Described sputtering DC source applies the power of 150w on nickel target, and vacuum is maintained at 1Pa；
Step 8) in described in DC arc plasma jet CVD equipment annealing temperature be 800 DEG C.
The invention have the advantage that the present invention uses Raney nickel plasma etching method to etch boron-doped diamond,
It is easier processed molding, during novel electron functional material moves towards actual application, has non-the normally off
The effect of key；This preparation method technique is simple, it is easy to implement, and target utilization rate is high, production cost is low, suitable
In large-scale popularization and application.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram after boron-doped diamond etching.
Detailed description of the invention
According to the structure that sample prepared in the present invention is carried out and property analysis, below will be to target response
The preferred forms of sputtering and annealing plasma etching boron-doped diamond is described in detail, and embodiment is adopted
With scientific instrument development center, Chinese Academy of Sciences Shenyang produce JGP-450a type dual chamber magnetron sputtering deposition system and
DC electric arc plasma chemical vapor deposition Diamond Film Equipment by Hebei province's laser Research Institute.Profit
Porous boron-doped diamond is prepared by said system.
Embodiment 1:
A kind of method of boron-doped diamond etching, this step is as follows:
1) installing, at coater negative electrode, the nickel target that purity is 99.99%, the thickness at nickel target is 5mm, diameter
For 60mm；Fixing boron-doped diamond sheet at anode, the distance between target base is 100mm；
2) open magnetron sputtering apparatus, successively start one-level mechanical pump and secondary molecules pumping vacuum, until sputtering
The back end vacuum of room is 1 × 10-4Pa；
3) it is passed through, to vacuum chamber, the argon that purity is 99.999%, vacuum is maintained at 1Pa, the stream of argon
Amount is 15sccm；
4) open shielding power supply, a pair nickel target apply electric current and voltage, makes power control at 150w,
Pre-sputtering 20 minutes, waits sputtering current and voltage stabilization；Open the baffle plate in substrate frame and start plated film, plated film
During substrate position fix；
5) the plated film time is 1 minute, after plated film terminates, closes the baffle plate in substrate frame, is then shut off sputtering
Power supply, stops being passed through sputter gas argon, fully opens gate valve, continue evacuation, be then shut off vacuum
System, system for the treatment of cools down backward vacuum chamber and is filled with air, when the air pressure of vacuum chamber is identical with external atmosphere pressure,
Open vacuum chamber, open sample and take out the boron-doped diamond sheet of nickel plating；
6) the boron-doped diamond sheet by nickel plating is placed in the sample stage of DC arc plasma jet CVD equipment
On support；
7) open power distribution cabinet, open electrical control cabinet, open water-cooling system and mechanical pump evacuation, when chamber press,
Pump pressure is all stable opens lobe pump degree of depth evacuation when below 3000Pa, until chamber pressure and pump pressure are
Below 0.1Pa, the flow being passed through hydrogen and argon, hydrogen and argon is 1.5L/min, waits that chamber pushes back liter
To 3000Pa, pump pressure is gone up to 13000Pa.
8) control switch in magnetic field is opened, and tune voltage is 6.0V, and arc power controls igniting and opens, and anneals 6 points
Clock, by controlling sample stage height, controls temperature at 800 DEG C；
9) close electrical control cabinet and power distribution cabinet after annealing terminates, after cooling down etc. deposition table, take out the mesh prepared
Mark product.
In order to the film surface making etching is uniform, change by changing plating time.According to above-mentioned preparation side
Step identical in method and condition, plating time chooses 30s, 60s, 2min respectively.
Fig. 1 gives the boron-doped diamond scanning electron microscope of optimum implementation etching.
The present invention proposes, by changing the method that nickel plating duration regulates and controls boron-doped diamond etching effect, i.e. to work as plating
When the nickel time is 1 minute, print etching effect is good.It is described by embodiment, person skilled
Substantially in without departing from present disclosure, spirit and scope, content as herein described can be modified or suitable
When change and combination, realize the present invention.Special needs to be pointed out is, all similar replacements and change right
Being apparent from for those skilled in the art, they are considered as being included in the spirit of the present invention, scope
With in content.
Claims (10)
1. the method for a boron-doped diamond etching, it is characterised in that using superhigh vacuum magnetron sputtering film-plating machine and DC arc plasma jet CVD equipment to prepare, this step is as follows:
1) at coater negative electrode, nickel target is installed, at anode fixed diamond sheet；
2) open to target magnetic control sputtering equipment, successively start one-level mechanical pump and secondary molecules pumping vacuum；
3) it is passed through argon to vacuum chamber；
4) open shielding power supply, a pair nickel target applies electric current and voltage, carries out pre-sputtering, wait sputtering current and voltage stabilization；Opening the baffle plate in substrate frame and start plated film, in coating process, substrate position is fixed；
5) after plated film terminates, close the baffle plate in substrate frame, it is then shut off shielding power supply, stops being passed through sputter gas argon, fully open gate valve, continue evacuation, being then shut off vacuum system, system for the treatment of cools down backward vacuum chamber and is filled with air, when the air pressure of vacuum chamber is identical with external atmosphere pressure, open vacuum chamber, open sample and take out the boron-doped diamond sheet of nickel plating；
6) the boron-doped diamond sheet of nickel plating is placed on the sample platform bracket of DC arc plasma jet CVD equipment；
7) open power distribution cabinet, open electrical control cabinet, open water-cooling system and mechanical pump evacuation, be passed through hydrogen and argon, wait that chamber pressure, pump pressure are gone up.
8) control switch in magnetic field is opened, annealing, by controlling sample stage height, controls temperature；
9) close electrical control cabinet and power distribution cabinet after annealing terminates, after cooling down etc. deposition table, take out the target product prepared.
Boron-doped diamond the most according to claim 1 etching method, it is characterised in that: step 2) in until the back end vacuum of sputtering chamber is 1 × 10-4Pa。
Boron-doped diamond the most according to claim 1 etching method, it is characterised in that: step 4) in the pre-sputtering time be 20 minutes；The plated film time is 1 minute.
The method of boron-doped diamond the most according to claim 1 etching, it is characterized in that: step 7) in, when chamber pressure, pump pressure are all stablized at below 3000Pa, open lobe pump degree of depth evacuation, during until chamber pressure and pump pressure are below 0.1Pa, it is passed through hydrogen and argon.
The method of boron-doped diamond the most according to claim 1 etching, it is characterised in that: step 7) in, chamber pushes back and rises to 3000Pa, and pump pressure is gone up to 13000Pa.
The method of boron-doped diamond the most according to claim 1 etching, it is characterised in that: step 8) in, magnetic field controls switch and opens, and tune voltage is 6.0V, and arc power controls igniting and opens, and anneals 6 minutes.
The method of boron-doped diamond the most according to claim 1 etching, it is characterised in that: the purity of described nickel target is 99.99%, and the thickness of target is 5mm, a diameter of 60mm.
The method of boron-doped diamond the most according to claim 1 etching, it is characterised in that: described argon, the purity of hydrogen is 99.999%, and in ultrahigh vacuum three target codeposition magnetron sputtering coater, the flow of argon is 15sccm；In DC arc plasma jet CVD equipment, the flow of hydrogen and argon is 1.5L/min.
The method of boron-doped diamond the most according to claim 1 etching, it is characterised in that: described sputtering DC source applies the power of 150w on nickel target, and vacuum is maintained at 1Pa.
Boron-doped diamond the most according to claim 1 etching method, it is characterised in that: step 8) in DC arc plasma jet CVD equipment annealing temperature be 800 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610237371.0A CN105887038A (en) | 2016-04-15 | 2016-04-15 | Method for etching boron-doped diamonds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610237371.0A CN105887038A (en) | 2016-04-15 | 2016-04-15 | Method for etching boron-doped diamonds |
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| CN105887038A true CN105887038A (en) | 2016-08-24 |
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| CN201610237371.0A Pending CN105887038A (en) | 2016-04-15 | 2016-04-15 | Method for etching boron-doped diamonds |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106971864A (en) * | 2017-04-24 | 2017-07-21 | 天津理工大学 | A kind of preparation method of the ultracapacitor based on nanoporous boron-doped diamond electrode |
| CN107267953A (en) * | 2017-05-18 | 2017-10-20 | 天津理工大学 | A kind of preparation method of carbon hollow ball and porous boron-doped diamond compound film sensor electrode |
| CN108315711A (en) * | 2018-02-26 | 2018-07-24 | 南京航空航天大学 | A kind of nanosecond laser substrate pretreated method improving boron-doped diamond electrode film base binding performance |
| CN108374160A (en) * | 2018-03-08 | 2018-08-07 | 南京元汀环境科技有限公司 | A kind of preparation method of high-quality titanium-based b-doped diamond film |
| CN108728798A (en) * | 2018-06-11 | 2018-11-02 | 哈尔滨工业大学 | A kind of processing method of diamond |
| CN111521656A (en) * | 2020-05-11 | 2020-08-11 | 中南大学 | High-sensitivity high-stability boron-doped diamond microelectrode and preparation method and application thereof |
| CN113897675A (en) * | 2021-09-15 | 2022-01-07 | 湖南新锋先进材料科技有限公司 | Diamond-doped particles and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106971864A (en) * | 2017-04-24 | 2017-07-21 | 天津理工大学 | A kind of preparation method of the ultracapacitor based on nanoporous boron-doped diamond electrode |
| CN107267953A (en) * | 2017-05-18 | 2017-10-20 | 天津理工大学 | A kind of preparation method of carbon hollow ball and porous boron-doped diamond compound film sensor electrode |
| CN108315711A (en) * | 2018-02-26 | 2018-07-24 | 南京航空航天大学 | A kind of nanosecond laser substrate pretreated method improving boron-doped diamond electrode film base binding performance |
| CN108315711B (en) * | 2018-02-26 | 2020-02-07 | 南京航空航天大学 | Nanosecond laser matrix pretreatment method for improving bonding performance of boron-doped diamond electrode film substrate |
| CN108374160A (en) * | 2018-03-08 | 2018-08-07 | 南京元汀环境科技有限公司 | A kind of preparation method of high-quality titanium-based b-doped diamond film |
| CN108728798A (en) * | 2018-06-11 | 2018-11-02 | 哈尔滨工业大学 | A kind of processing method of diamond |
| CN111521656A (en) * | 2020-05-11 | 2020-08-11 | 中南大学 | High-sensitivity high-stability boron-doped diamond microelectrode and preparation method and application thereof |
| CN113897675A (en) * | 2021-09-15 | 2022-01-07 | 湖南新锋先进材料科技有限公司 | Diamond-doped particles and preparation method and application thereof |
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