CN108823550A - A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film - Google Patents

A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film Download PDF

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Publication number
CN108823550A
CN108823550A CN201810578256.9A CN201810578256A CN108823550A CN 108823550 A CN108823550 A CN 108823550A CN 201810578256 A CN201810578256 A CN 201810578256A CN 108823550 A CN108823550 A CN 108823550A
Authority
CN
China
Prior art keywords
sang shi
ornaments
diamond film
sang
shi
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810578256.9A
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Chinese (zh)
Inventor
何金鑫
吕反修
黑立富
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Jin Xin Fung Li Jewelry Co Ltd
Original Assignee
Shenzhen Jin Xin Fung Li Jewelry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen Jin Xin Fung Li Jewelry Co Ltd filed Critical Shenzhen Jin Xin Fung Li Jewelry Co Ltd
Priority to CN201810578256.9A priority Critical patent/CN108823550A/en
Publication of CN108823550A publication Critical patent/CN108823550A/en
Priority to PCT/IB2019/000641 priority patent/WO2019234496A2/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical 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
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only
    • AHUMAN NECESSITIES
    • A44HABERDASHERY; JEWELLERY
    • A44CPERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
    • A44C17/00Gems or the like
    • AHUMAN NECESSITIES
    • A44HABERDASHERY; JEWELLERY
    • A44CPERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
    • A44C27/00Making jewellery or other personal adornments
    • A44C27/001Materials for manufacturing jewellery
    • A44C27/005Coating layers for jewellery
    • A44C27/007Non-metallic coatings
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0227Pretreatment of the material to be coated by cleaning or etching
    • C23C16/0245Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0254Physical treatment to alter the texture of the surface, e.g. scratching or polishing

Abstract

A kind of not Sang Shi ornaments, Sang Shi jewelry surface is not coated with diamond film.A method of diamond film being plated in not Sang Shi jewelry surface, this method comprises the following steps:Step 1:Ultrasonic grinding pretreatment is carried out to not Sang Shi ornaments in Nano diamond powder suspension;Step 2:It will not take out Sang Shi ornaments, and be cleaned from the Nano diamond powder suspension;Step 3:It incites somebody to action and is kept in the not preset conformal sample stage of Sang Shi ornaments indentation;Step 4:Sang Shi ornaments it will be placed in diamond film deposition furnace together together with the conformal sample stage and carry out corona treatment;Step 5:It is passed through methane, carries out diamond film deposition in situ.Surface of the invention is coated with the not Sang Shi ornaments of diamond film, can greatly improve its surface hardness, this improves the scratch resistant performances of not Sang Shi while keeping not Sang Shi optical property.

Description

A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film
Technical field
The present invention relates to Jewelry Accessories fields, more particularly to a kind of not Sang Shi ornaments, and the invention further relates to one kind in not mulberry The method of stone jewelry surface plating diamond film.
Background technique
The internal structure of Sang Shi, numerical value, appearance be not all shockingly similar to diamond, even if being difficult to point with diamond pen detection Distinguish, but Mo Sangshi can glitter brighter than diamond, fire coloured silk is more pleasantly surprised, while price also than diamond it is cheap very much, Therefore, Mo Sangshi is also usually used to be processed into ornaments.
But the hardness of Mo Sangshi is lower than diamond (diamond), therefore adhesion strength is more very different than diamond.
Summary of the invention
The present invention proposes a kind of with high surface hardness for the not poor technical problem of Sang Shi adhesion strength Not Sang Shi ornaments, in addition, the invention also provides a kind of methods in not Sang Shi jewelry surface plating diamond film.
It is a kind of that Sang Shi ornaments, the not Sang Shi jewelry surface are not coated with diamond film.
Further, the average grain size of the diamond film is 100nm-200nm.
A method of diamond film being plated in not Sang Shi jewelry surface, is included the following steps:Step 1:In Nano diamond Ultrasonic grinding pretreatment is carried out to not Sang Shi ornaments in powder suspension;Step 2:Will not Sang Shi ornaments from the Nano diamond It takes out, and is cleaned in powder suspension;Step 3:It incites somebody to action and is kept in the not preset conformal sample stage of Sang Shi ornaments indentation; Step 4:It will Sang Shi ornaments be placed in diamond film deposition furnace together at progress plasma together with the conformal sample stage Reason;Step 5:It is passed through methane, carries out diamond film deposition in situ.
Preferably, the granularity of Nano diamond powder is 5nm- in the suspension of Nano diamond powder described in step 1 200nm, the concentration of Nano diamond powder is 5%-20% in the Nano diamond powder suspension.
Preferably, the ultrasonic grinding pretreated time is 2h-6h.
Preferably, the material of conformal sample stage described in step 3 is fine copper or graphite.
Preferably, the recess portion for keeping not Sang Shi ornaments is provided in the conformal sample stage, it will not in step 3 The pressure that Sang Shi ornaments are pressed into the recess portion is 50Kgf-250Kgf.
Preferably, corona treatment described in step 4 uses Dc arc plasma jet CVD or microwave plasma Injection.
Preferably, the temperature of the corona treatment is 700 DEG C -1000 DEG C, and the time of the corona treatment is 5min-30min。
Preferably, the concentration of methane described in step 5 is 0.5%-10%, and the pressure of the cvd furnace is 3kPa- 20kPa, sedimentation time 5min-120min.
Surface of the invention is coated with the not Sang Shi ornaments of diamond film, can be while keeping not Sang Shi optical property, greatly The earth promotes its surface hardness, and this improves the scratch resistant performances of not Sang Shi.In addition, by means of the invention it is also possible to real Sang Shi jewelry surface does not obtain the diamond film coating of even compact, excellent in optical properties now, improves not Sang Shi ornaments Surface hardness.
Detailed description of the invention
Fig. 1 is surface A FM (atomic force microscope) shape appearance figure that surface is coated with that the not mulberry of diamond film is bored;
Fig. 2 is typical Raman (Raman) spectrogram that surface is coated with that the not mulberry of diamond film is bored;
Fig. 3 is not plate the scratch of not mulberry brill of diamond film aobvious after carrying out anti-diamond pressing delineation capacity experimental Figure observed by amplifying 100 times under micro mirror;
Fig. 4 is to plate the scratch of not mulberry brill of diamond film in microscope after carrying out anti-diamond pressing delineation capacity experimental Figure observed by lower 200 times of amplification;
Fig. 5 is the structural schematic diagram of conformal sample stage used in the present invention.
Specific embodiment
Referring to Fig. 1 to Fig. 5, the present invention is described in detail.
A kind of not Sang Shi ornaments, Sang Shi jewelry surface is not coated with diamond film.By taking Mo Sang is bored as an example, referring to Fig.1, the Buddha's warrior attendant The not mulberry of stone membrane coat bores the pattern observed of the sample surfaces under AFM (atomic force microscope), and coating structure is fine and close, equal Even, average grain size is 100nm-200nm or so.
Referring to Fig. 2, it is seen that be located at 1331cm-1Diamond Raman (Raman) characteristic peak.Positioned at 1120cm-1Neighbouring dissipates Unrestrained peak is related with the grain size of diamond film, is a very tiny presentation of crystal grain.It is shown in the appearance at this peak and Fig. 1 micro- Little crystal grain is consistent.
Referring to Fig. 3, Fig. 4, in the not Sang Shi ornaments for having diamond film to surface and not no not Sang Shi ornaments of diamond film When carrying out the experiment of anti-diamond pressing delineation ability under the normal pressure of maximum 20N, in scoring process, normal pressure is (real by zero Pretightning force is 0.02N on border) it is gradually increased to 20N, during this period in (1 minute), the distance streaked is 2mm.
Wherein, the not Sang Shi ornaments of diamond film do not occur about (to amplify from optical microscopy in 8N or more Multiple 100) photo is clearly visible scratch, and a series of lateral sharp cracks occurs, and under equal conditions, there is diamond film on surface Not Sang Shi ornaments there is no obvious scratch.For the not Sang Shi ornaments that there is diamond film on surface, close to maximum pressure (20N) Shi Caicong optical microscopy (amplification factor 200) photo can be seen that diamond film just by pressure break, the mark of brittle fracture occurs As breach is very smooth, and as being cut knife, and film opens, and rolls.Therefore, can be illustrated by experiment, surface has diamond The not Sang Shi ornaments of film are substantially at pressure sufficiently large (close to 20N) just by pressure break.Compared to the decorations of no plating diamond film For product, adhesion strength is greatly improved.
The method in not Sang Shi jewelry surface plating diamond film is illustrated below.
This method comprises the following steps:Step 1:Ultrasound is carried out to not Sang Shi ornaments in Nano diamond powder suspension Grinding pretreatment.Wherein, in Nano diamond powder suspension the granularity of Nano diamond powder in 5nm-200nm, nanogold The concentration of Nano diamond powder is 5%-20% in hard rock powder suspension, and the ultrasonic grinding pretreated time is 2h-6h.It should The purpose of step mainly for improve diamond film deposition Enhancing Nucleation Density so that the Enhancing Nucleation Density of diamond film be greater than 1010cm-2
After ultrasonic grinding pre-processes, in step 2:It will Sang Shi ornaments not taken from Nano diamond powder suspension Out, it and is cleaned, wherein cleaning is successively cleaned by ultrasonic using deionized water and dehydrated alcohol, is dried up through cold wind.
Not Sang Shi ornaments after ultrasonic grinding pre-processes and cleans, in step 3:It will the indentation of Sang Shi ornaments not set in advance It is kept in fixed conformal sample stage.Wherein, by taking Mo Sang is bored as an example, in order to keep not, mulberry brill can be in conformal sample stage referring to Fig. 5 In be provided with recess portion 111 for keeping not Sang Shi ornaments, which is in back taper, and the depth H of recess portion 111 is about It is the 4/5 of not mulberry drilling depth, substantially 96 ° of the cone angle R of back taper, can permit 0 ° -- 2 ° of error, for the ease of Mo Sang brill The material of indentation, conformal sample stage is slightly softer using fine copper or graphite etc. and has the material of good thermal conductivity.Mo Sang Boring can be pressed into the recess portion of conformal sample stage by applying the pressure of 50Kgf-250Kgf.
It is pre-processed by ultrasonic grinding, and after not mulberry bored being pressed into the recess portion of conformal sample stage, it in step 4, will not mulberry Drill ornaments are placed in diamond film deposition furnace together together with conformal sample stage and carry out corona treatment.In step 4, direct current Arc-plasma sprays (DC Arc Plasma Jet) CVD, and microwave plasma sprays CVD (MWCVD) and HF CVD (HFCVD) diamond film coating that diamond film depositions method is used equally for Mo Sang to bore such as.But HF CVD is living due to gas Change degree is not high, causes atomic hydrogen concn too low, for the diamond film coating layer ratio for figuring for having favorable optical performance It is more difficult.Therefore, in step 4, corona treatment is sprayed using Dc arc plasma jet CVD or microwave plasma. The temperature of corona treatment is 700 DEG C -1000 DEG C, and the time of corona treatment is 5min-30min.Appointed with completely removing What remains in organic root ball (from Nano diamond powder suspension) on Mo Sang brill surface to deposition of diamond thin films It influences, and activates the surface state that not mulberry bores sample, conducive to the uniform deposition of diamond film and the adhesive force of raising diamond film.
After completing corona treatment, in steps of 5:It is passed through methane, carries out diamond film deposition in situ immediately.In the step In rapid, the concentration of methane is 0.5%-10%, and the surface temperature that Mo Sang is bored is 700 DEG C -1000 DEG C, and the pressure of cvd furnace is set as 3kPa-20kPa, sedimentation time 5min-120min.
It is 10 minutes cooling after the completion of deposition, that is, it can be taken off the sample that the not mulberry of plated film is bored.
The example for the diamond film plated film for taking the not mulberry that diameter is 6.5mm to bore (1 carat) further below is illustrated.
Sample ultrasonic grinding 3h in 30nm diamond dust suspension will not bored by mulberry first.
Sample taking-up will not bored by mulberry, cleaned up.
In 150kg power indentation height is 30mm, prefabricated back taper is cheated on the conformal sample stage surface of copper that diameter is 50mm (95 ° of cone angle).
It will mulberry brill sample not be put into dc arc plasma CVD diamond film deposition furnace, in argon/hydrogen plasma Handle 5 minutes (Ar:3slm;H2:8slm;Chamber pressure:3-6kPa;Plasma torch electric current:190A;Voltage:97V).Then to etc. It is passed through methane in gas ions, flow 50sccm-240sccm, 700 DEG C -1000 DEG C of sample surface temperature, time 5min- 30min.Electric current is cut off, diamond film deposition is stopped, the cooling not mulberry that can be taken off plated film after ten minutes bores sample.
The not mulberry of the sample and non-coating that are bored by the not mulberry for being coated with diamond film coating layer that this method obtains is bored outer Sight is compared, and can not see that diamond film coating has an impact to the optical property (heat color) that not mulberry is bored.In addition, the diamond film applies The not mulberry of layer bores the pattern observed of the sample surfaces under AFM (atomic force microscope), and coating structure is fine and close, uniform, average Crystallite dimension is 100nm-200nm or so.
The above description is only an embodiment of the present invention, not limits the scope of the invention, all to be said using the present invention The equivalent structure or equivalent process transformation that bright book content is done, are directly or indirectly used in other correlative technology fields, It should be included in scope of patent protection of the invention.

Claims (10)

1. a kind of not Sang Shi ornaments, it is characterised in that:The not Sang Shi jewelry surface is coated with diamond film.
2. a kind of not Sang Shi ornaments according to claim 1, it is characterised in that:The average grain size of the diamond film For 100nm-200nm.
3. a kind of method in not Sang Shi jewelry surface plating diamond film, which is characterized in that include the following steps:
Step 1:Ultrasonic grinding pretreatment is carried out to not Sang Shi ornaments in Nano diamond powder suspension;
Step 2:It will not take out Sang Shi ornaments, and be cleaned from the Nano diamond powder suspension;
Step 3:It incites somebody to action and is kept in the not preset conformal sample stage of Sang Shi ornaments indentation;
Step 4:Sang Shi ornaments it will be placed in diamond film deposition furnace together together with the conformal sample stage and carry out plasma Body processing;
Step 5:It is passed through methane, carries out diamond film deposition in situ.
4. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 3, which is characterized in that step The granularity of Nano diamond powder is 5nm-200nm, the nano-diamond powder in the suspension of Nano diamond powder described in 1 The concentration of Nano diamond powder is 5%-20% in last suspension.
5. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 3, which is characterized in that described The ultrasonic grinding pretreated time is 2h-6h.
6. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 3 or 6, which is characterized in that The material of conformal sample stage described in step 3 is fine copper or graphite.
7. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 6, which is characterized in that described Be provided with the recess portion for keeping not Sang Shi ornaments in conformal sample stage, in step 3 will not the indentation of Sang Shi ornaments it is described recessed The pressure in portion is 50Kgf-250Kgf.
8. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 3, which is characterized in that step Corona treatment described in 4 is sprayed using Dc arc plasma jet CVD or microwave plasma.
9. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 8, which is characterized in that described The temperature of corona treatment is 700 DEG C -1000 DEG C, and the time of the corona treatment is 5min-30min.
10. a kind of method in not Sang Shi jewelry surface plating diamond film according to claim 3, which is characterized in that step The concentration of methane described in rapid 5 is 0.5%-10%, and the pressure of the cvd furnace is 3kPa-20kPa, sedimentation time 5min- 120min。
CN201810578256.9A 2018-06-07 2018-06-07 A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film Pending CN108823550A (en)

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CN201810578256.9A CN108823550A (en) 2018-06-07 2018-06-07 A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film
PCT/IB2019/000641 WO2019234496A2 (en) 2018-06-07 2019-08-07 Moissanite decorative product, and method of coating surface of same with diamond film

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CN201810578256.9A CN108823550A (en) 2018-06-07 2018-06-07 A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019234496A3 (en) * 2018-06-07 2021-10-07 深圳市金鑫丰利珠宝首饰有限公司 Moissanite decorative product, and method of coating surface of same with diamond film
WO2023035429A1 (en) * 2021-09-13 2023-03-16 吕反修 Method for depositing diamond film coating on surface of moissanite

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CN108823550A (en) * 2018-06-07 2018-11-16 深圳市金鑫丰利珠宝首饰有限公司 A method of not Sang Shi ornaments and not Sang Shi jewelry surface plate diamond film

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019234496A3 (en) * 2018-06-07 2021-10-07 深圳市金鑫丰利珠宝首饰有限公司 Moissanite decorative product, and method of coating surface of same with diamond film
WO2023035429A1 (en) * 2021-09-13 2023-03-16 吕反修 Method for depositing diamond film coating on surface of moissanite
WO2023035287A1 (en) * 2021-09-13 2023-03-16 吕反修 Diamond film coated ornament and preparation method for diamond film coating

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WO2019234496A2 (en) 2019-12-12

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Application publication date: 20181116