CN108411276A - A kind of crystal seed implantation methods of cvd diamond thick film - Google Patents
A kind of crystal seed implantation methods of cvd diamond thick film Download PDFInfo
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- CN108411276A CN108411276A CN201810307217.5A CN201810307217A CN108411276A CN 108411276 A CN108411276 A CN 108411276A CN 201810307217 A CN201810307217 A CN 201810307217A CN 108411276 A CN108411276 A CN 108411276A
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- Prior art keywords
- molybdenum
- crystal seed
- molybdenum substrate
- implantation methods
- thick film
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or polishing
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A kind of crystal seed implantation methods of cvd diamond thick film, are related to diamond field, comprise the following steps：The surface of molybdenum substrate is pre-processed first, diadust grinding will be added in molybdenum substrate top surface on polishing machine when processing, the molybdenum carbide of molybdenum underlayer surface is removed, make the smooth color light no marking in surface, it is required that there is no molybdenums and molybdenum carbide to be layered, then fine grinding is carried out to molybdenum substrate, fine grinding is added varigrained diadust with hard metal tip and is ground.Crystal seed implantation methods of the present invention compensate for the still nonstandard blank of cvd diamond thick film manufacturing method in the prior art, and the diamond thick-film prepared has the characteristics that reliable and stable and deposition rate is high, it is entirely capable of meeting actual demand, technical solution of the present invention is simple, is suitble to large-scale promotion and application.
Description
Technical field
The present invention relates to diamond fields, and in particular to a kind of crystal seed implantation methods of cvd diamond thick film.
Background technology
Known, diamond is one of special material existing for nature, integrates plurality of advantages, such as：Hardness highest,
Elasticity modulus is maximum, highest thermal conductivity, very big with excellent field emission characteristics, energy gap, is a kind of development prospect
Quite good semi-conducting material；It is also classic optical window material, from ultraviolet to the very wide of far infrared or even microwave
There is excellent through performance in electromagnetic regime.
But traditional diamond（It is natural and artificial）Majority is presented with bulk forms, this also limits its application.Buddha's warrior attendant
Stone thin film physics are chemically excellent, and cost is low compared with natural diamond, can prepare various geometries, be to size theoretically
There is no limit, have wide practical use in industrial circles such as electronics, optics, machineries, the various advantages of film collection of diamond
, or even scientist points out：Diamond thin is after the Stone Age, the Bronze Age, steel epoch, silicon materials epoch
Since the 5th generation new material.
Diamond thin is generated using CVD method at present, and cvd diamond mainly has following typical feature：
1, large area：CVD technology is capable of providing large area, the excellent diamonds that natural mineral products are unable to reach；
2, large volume：With the diamond phase ratio of high temperature and high pressure method production, the performance of cvd diamond wants more advantageous, due to having
Bulk solid feature, application field, range etc. are much broader, really open the new era of the comprehensive application of diamond；
3, film spreadability：CVD method can generate diamond thin, coating, further increase the application of cvd diamond technology
Field etc..
Cvd diamond is although moved towards market, and technology is there is still a need for further increasing, especially for CVD gold
The crystal seed implantation methods of diamond thick film, it would be highly desirable to specification, therefore it provides a kind of crystal seed implantation methods of cvd diamond thick film are just shown
It obtains particularly important.
Invention content
Insufficient present in background technology to overcome, the present invention provides a kind of crystal seed plantation sides of cvd diamond thick film
Method has reliable and stable and deposition rate height etc. special using diamond thick-film prepared by crystal seed implantation methods of the present invention
Point is entirely capable of meeting actual demand.
To realize that goal of the invention as described above, the present invention use technical solution as described below：
A kind of crystal seed implantation methods of cvd diamond thick film, the crystal seed implantation methods specifically comprise the following steps：
The first step first pre-processes the surface of molybdenum substrate, and gold will be added in molybdenum substrate top surface on polishing machine when processing
Hard rock micro mist is ground, and the molybdenum carbide of molybdenum underlayer surface is removed, the smooth color light no marking in surface is made, it is desirable that there is no molybdenum and
Molybdenum carbide is layered；
Second step takes the next step, and fine grinding is carried out to molybdenum substrate：Fine grinding hard metal tip be added varigrained diadust into
Row grinding, concrete operation method are：
A, 1 carat of W30-70 diadust is taken uniformly to be sprinkling upon molybdenum substrate surface first, instilling 1~5 with rubber dropper drips, will
Hard metal tip, which is pressed in above molybdenum substrate, is lightly ground 5~20min, then with water that surface clean is clean, observes surface appearance,
To check whether hard alloy has scar if there are cut, if any the hard alloy more to renew；
B, repeat top-operation twice, use W40-60, W30-40 to grind respectively, it is equal to reach surface crystal seed after grinding twice
It is even, no marking；
C, it takes 1 carat of W10-20 diadust to be uniformly sprinkling upon molybdenum substrate surface, is instilled and 1~5 dripped with rubber dropper, with hard
Matter alloy sheet is ground, until molybdenum substrate surface is smooth, the uniform no marking of crystal seed；
D, w10-20 diadusts are added with flannelette package hard metal tip to be ground, it is brilliant until molybdenum substrate surface light
The uniform no marking of kind；
E, w5-10 diadusts are added with flannelette package hard metal tip to be ground, until molybdenum substrate surface light, crystal seed
Uniform no marking；
F, molybdenum substrate surface is cleaned, surface trowel used for plastering dirt is cleaned up by ground molybdenum substrate with cleaning solution first, is then taken
Appropriate amount of deionized water pours into cleaning box, box is put into rinse bath, then molybdenum substrate top surface is immersed cleaning box, requires molybdenum to serve as a contrast at this time
Bottom surface cannot encounter cassette bottom, with ultrasonic cleaning, then use alcohol rinse molybdenum substrate surface and electricity consumption blowing drying；
G, give cleaned molybdenum substrate to Quality Inspector and carry out surface examination, it is qualified after 1~10min of electricity consumption blowing again, then
Preservation is sealed with preservative film.
The crystal seed implantation methods of the cvd diamond thick film, diadust is W50-70 Buddha's warrior attendants in the first step
Stone micro mist.
The crystal seed implantation methods of the cvd diamond thick film, hard metal tip is the hard of Φ 35 × 2 in the second step
Matter alloy sheet.
The crystal seed implantation methods of the cvd diamond thick film, in the second step dosage of deionized water be 100ml~
300ml。
The crystal seed implantation methods of the cvd diamond thick film, in the second step time of ultrasonic cleaning be 3~
10min。
The crystal seed implantation methods of the cvd diamond thick film, the time that the second step is ground twice adds up to 20~
50min。
Using technical solution as described above, the present invention has superiority as described below：
Diamond thick-film prepared by crystal seed implantation methods of the present invention has the characteristics that reliable and stable and deposition rate is high, complete
Actual demand all can be met, technical solution of the present invention is simple, is suitble to large-scale promotion and application.
Specific implementation mode
The present invention can be explained in more detail by the following examples, the invention is not limited in the following examples；
A kind of crystal seed implantation methods of cvd diamond thick film of the present invention, the crystal seed implantation methods specifically include as follows
Step：
The first step first pre-processes the surface of molybdenum substrate, and molybdenum substrate top surface will be added on polishing machine when processing
W50-70 diadusts are ground, and the molybdenum carbide of molybdenum underlayer surface is removed, makes the smooth color light no marking in surface, it is desirable that no
There are molybdenum and molybdenum carbide layering, this step should be noted that molybdenum surface is shaded, and molybdenum carbide surface is shinny, such as there is secretly bright interlock
Then show substrate surface there are lamination be defective work；
Second step takes the next step, and fine grinding is carried out to molybdenum substrate：Varigrained gold is added with the hard metal tip of Φ 35 × 2 in fine grinding
Hard rock micro mist is ground, and concrete operation method is：
A, 1 carat of W30-70 diadust is taken uniformly to be sprinkling upon molybdenum substrate surface first, instilling 1~5 with rubber dropper drips, will
Hard metal tip, which is pressed in above molybdenum substrate, is lightly ground 5~20min, then with water that surface clean is clean, observes surface appearance,
To check whether hard alloy has scar if there are cut, if any the hard alloy more to renew；
B, repeat top-operation twice, use W40-60, W30-40 to grind respectively, be co-mulled and made into 20~50min twice, reach table
Face crystal seed is uniform, no marking；
C, it takes 1 carat of W10-20 diadust to be uniformly sprinkling upon molybdenum substrate surface, is instilled and 1~5 dripped with rubber dropper, with hard
Matter alloy sheet is ground, until molybdenum substrate surface is smooth, the uniform no marking of crystal seed；
D, w10-20 diadusts are added with flannelette package hard metal tip to be ground, it is brilliant until molybdenum substrate surface light
The uniform no marking of kind；
E, w5-10 diadusts are added with flannelette package hard metal tip to be ground, until molybdenum substrate surface light, crystal seed
Uniform no marking；
F, molybdenum substrate surface is cleaned, surface trowel used for plastering dirt is cleaned up by ground molybdenum substrate with cleaning solution first, is then taken
The deionized water of 100ml~300ml pours into cleaning box, box is put into rinse bath, then molybdenum substrate top surface is immersed cleaning box, this
Shi Yaoqiu molybdenums substrate surface cannot encounter cassette bottom, with 3~10min of ultrasonic cleaning, then use alcohol rinse molybdenum substrate surface simultaneously
Electricity consumption blowing drying；
G, give cleaned molybdenum substrate to Quality Inspector and carry out surface examination, it is qualified after 1~10min of electricity consumption blowing again, then
Preservation is sealed with preservative film.
The present invention should meet following requirement when specific operation：
1, first surface and side should be polished before powder grinding on molybdenum BOB(beginning of block) clean, surface will reach bright and clean smooth, and no marking is small
Hole, side is polished to surrounding even uniform with sand paper.Molybdenum block bottom surface will also be handled totally to prevent bottom surface from having impurity to cause heat conduction
It is uneven and influence production and be normally carried out.（Note：Side and four weekly assemblies grow one layer of diamond-like, meeting to molybdenum block after a period of use
The heat conduction of molybdenum block in production process is influenced, molybdenum block should carry out blasting treatment after often producing 3~5 times, the eka-gold through side and surrounding
Hard rock spray is fallen, and is subject to and exposes molybdenum block background color.）
2, it has to carry out by the step of grinding technics requirement in molybdenum block process of lapping, ensures all to reach grinding technics per procedure
Required standard, previous procedure, which is not up to standard, cannot carry out the operation of next procedure, cannot absolutely occur leak process or
Single process grinds underproof phenomenon.
3, according to requiring the various processes of diaphragm thickness to have corresponding change, this requires the grinding of molybdenum block is whole
Can a very important link in a production process be the basis that produce diaphragm quality.The grinding of molybdenum block must root
Corresponding adjustment etc. is made according to actual conditions.
4, the grinding of molybdenum block terminates to fill in grinding technics list after the assay was approved, and grinding technics list wants realistic when filling in
The information of false mistake cannot be filled in by recording entire process of lapping absolutely, because grinding technics single pair is in entirely production work
The formulation of skill suffers from critically important reference value with the analysis and summary for improving and producing.
The present invention is when specific operation it should be noted that following item：
1, diamond-like of the edges of substrate in the 20mm of upper surface is knocked out before grinding, lower surface is ground with 400 mesh waterproof abrasive papers
It is flat；
2, add water less as possible in process of lapping, in case hypervolia washes out bortz powder, in addition, carefully to listen the sound of grinding
Sound should stop if there is sharp sound, washes with water at once, see whether surface scratches；
3, to ensure the clean of hand, then be cleaned again, in order to avoid leave watermark；
4, the substrate preserved is sure not to contact upper surface with hand；
5, new molybdenum is answered for the first time using in characteristics such as density and the thermal conductivity for not knowing about molybdenum block by changing the methods of tin silk amount
So that molybdenum deblocking temperature is maintained at the minimum of suitable for producing as possible to prevent the unexpected high temperature of molybdenum block and is destroyed；
6, molybdenum block pre-treatment polishes that be likely to result in surface after using certain number not smooth enough only on polishing machine, this
When molybdenum block should be placed on carry out polishing on surface grinding machine it is levelling with ensure production diaphragm uniformity；
7, molybdenum block lead angle after polishing certain number can become smaller, when being possible to influence shutdown when lead angle width is less than 1mm
The size that the quality of skinning at this time should require lead angle vehicle to molybdenum block size.
Part not in the detailed description of the invention is the prior art.
The embodiment selected herein for the open purpose of the present invention, is presently considered to be suitable, still, Ying Liao
Solution belongs to all changes and the improvement of the embodiment in this design and invention scope the present invention is intended to include all.
Claims (6)
1. a kind of crystal seed implantation methods of cvd diamond thick film, it is characterized in that：The crystal seed implantation methods specifically include following step
Suddenly：
The first step first pre-processes the surface of molybdenum substrate, and gold will be added in molybdenum substrate top surface on polishing machine when processing
Hard rock micro mist is ground, and the molybdenum carbide of molybdenum underlayer surface is removed, the smooth color light no marking in surface is made, it is desirable that there is no molybdenum and
Molybdenum carbide is layered；
Second step takes the next step, and fine grinding is carried out to molybdenum substrate：Fine grinding hard metal tip be added varigrained diadust into
Row grinding, concrete operation method are：
A, 1 carat of W30-70 diadust is taken uniformly to be sprinkling upon molybdenum substrate surface first, instilling 1~5 with rubber dropper drips, will
Hard metal tip, which is pressed in above molybdenum substrate, is lightly ground 5~20min, then with water that surface clean is clean, observes surface appearance,
To check whether hard alloy has scar if there are cut, if any the hard alloy more to renew；
B, repeat top-operation twice, use W40-60, W30-40 to grind respectively, it is equal to reach surface crystal seed after grinding twice
It is even, no marking；
C, it takes 1 carat of W10-20 diadust to be uniformly sprinkling upon molybdenum substrate surface, is instilled and 1~5 dripped with rubber dropper, with hard
Matter alloy sheet is ground, until molybdenum substrate surface is smooth, the uniform no marking of crystal seed；
D, w10-20 diadusts are added with flannelette package hard metal tip to be ground, it is brilliant until molybdenum substrate surface light
The uniform no marking of kind；
E, w5-10 diadusts are added with flannelette package hard metal tip to be ground, until molybdenum substrate surface light, crystal seed
Uniform no marking；
F, molybdenum substrate surface is cleaned, surface trowel used for plastering dirt is cleaned up by ground molybdenum substrate with cleaning solution first, is then taken
Appropriate amount of deionized water pours into cleaning box, box is put into rinse bath, then molybdenum substrate top surface is immersed cleaning box, requires molybdenum to serve as a contrast at this time
Bottom surface cannot encounter cassette bottom, with ultrasonic cleaning, then use alcohol rinse molybdenum substrate surface and electricity consumption blowing drying；
G, give cleaned molybdenum substrate to Quality Inspector and carry out surface examination, it is qualified after 1~10min of electricity consumption blowing again, then
Preservation is sealed with preservative film.
2. the crystal seed implantation methods of cvd diamond thick film according to claim 1, it is characterized in that：It is golden in the first step
Hard rock micro mist is W50-70 diadusts.
3. the crystal seed implantation methods of cvd diamond thick film according to claim 1, it is characterized in that：It is hard in the second step
Matter alloy sheet is the hard metal tip of Φ 35 × 2.
4. the crystal seed implantation methods of cvd diamond thick film according to claim 1, it is characterized in that：In the second step
The dosage of ionized water is 100ml~300ml.
5. the crystal seed implantation methods of cvd diamond thick film according to claim 1, it is characterized in that：Surpass in the second step
The time of sound wave cleaning is 3~10min.
6. the crystal seed implantation methods of cvd diamond thick film according to claim 1, it is characterized in that：The second step is twice
The time of grinding adds up to 20~50min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810307217.5A CN108411276B (en) | 2018-04-08 | 2018-04-08 | A kind of crystal seed implantation methods of cvd diamond thick film |
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| CN201810307217.5A CN108411276B (en) | 2018-04-08 | 2018-04-08 | A kind of crystal seed implantation methods of cvd diamond thick film |
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| CN108411276A true CN108411276A (en) | 2018-08-17 |
| CN108411276B CN108411276B (en) | 2019-12-03 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004034667A1 (en) * | 2004-07-18 | 2006-02-09 | Heraeus Quarzglas Gmbh & Co. Kg | Producing synthetic diamond particles comprises exposing hydrogen and fluidized carbon seed particles to an energy source |
| US20100166635A1 (en) * | 2008-12-31 | 2010-07-01 | Chien-Min Sung | Interrupted Diamond Growth |
| CN104164659A (en) * | 2014-08-08 | 2014-11-26 | 上海交通大学 | Preparation method of seed crystal-free fine monocrystal diamond micro-powder |
| CN106011776A (en) * | 2016-07-14 | 2016-10-12 | 上海开山中夏节能科技有限公司 | Method for planting diamond crystallites on surface of titanium tube |
| CN107419329A (en) * | 2017-05-22 | 2017-12-01 | 北京科技大学 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
-
2018
- 2018-04-08 CN CN201810307217.5A patent/CN108411276B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004034667A1 (en) * | 2004-07-18 | 2006-02-09 | Heraeus Quarzglas Gmbh & Co. Kg | Producing synthetic diamond particles comprises exposing hydrogen and fluidized carbon seed particles to an energy source |
| US20100166635A1 (en) * | 2008-12-31 | 2010-07-01 | Chien-Min Sung | Interrupted Diamond Growth |
| CN104164659A (en) * | 2014-08-08 | 2014-11-26 | 上海交通大学 | Preparation method of seed crystal-free fine monocrystal diamond micro-powder |
| CN106011776A (en) * | 2016-07-14 | 2016-10-12 | 上海开山中夏节能科技有限公司 | Method for planting diamond crystallites on surface of titanium tube |
| CN107419329A (en) * | 2017-05-22 | 2017-12-01 | 北京科技大学 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
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