CN1769226B - Wearing layer-possessing mould core and its preparation method - Google Patents
Wearing layer-possessing mould core and its preparation method Download PDFInfo
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- CN1769226B CN1769226B CN2004100521575A CN200410052157A CN1769226B CN 1769226 B CN1769226 B CN 1769226B CN 2004100521575 A CN2004100521575 A CN 2004100521575A CN 200410052157 A CN200410052157 A CN 200410052157A CN 1769226 B CN1769226 B CN 1769226B
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- wearing layer
- die
- layer
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- mold
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The invention provides a die kernel with wearing coat used for pressing glass product, which contains a die kernel matrix with pressing panel; and a wearing coat covering the pressing panel, whose thickness is within range of 20nm to 200nm. The wearing coat can improve the wear resistance of said die kernel effectively. The invention also provides a method for preparation of die kernel with said wearing coat.
Description
[technical field]
The present invention relates to a kind of die that is used for mold pressing opticglass, relate in particular to a kind of die and preparation method thereof with wearing layer.
[background technology]
Die is widely used in the compression molding processing procedure, particularly make the opticglass product, as aspheric surface glass lens, globe lens, prism etc., adopt direct compression molding (Direct Press-molding) but technology direct production opticglass product, need not subsequent process steps such as polishing, polishing, can enhance productivity greatly and output, and good product quality.But directly compression molding method requires very high for the chemical stability of die, thermal shock resistance, physical strength, surface flatness etc.So in fact the development of compression molding technology depends primarily on die material and die improvement of Manufacturing Technology.Die for compression molding generally has following requirement:
A. when high temperature, has good rigidity, anti-mechanical impact strength and enough hardness;
B. do not crack and be out of shape reaching under the thermal shocking of rapid heating refrigerative die repeatedly;
C. chemical reaction does not take place with opticglass in the die surface when high temperature, does not adhere to glass;
D., high temperature oxidation does not take place;
E. good processability easily is processed into the profile of high precision and high surface finish;
F. cost is low.
The tradition die adopts stainless steel or refractory alloy as the die material mostly, and high temperature oxidation takes place this die easily, under thermal shocking effect repeatedly, grain growth can take place, thus die surface roughen, adhesive glass.
For addressing the above problem, nonmetal and superhard alloy is used to die.According to reports, silicon carbide (SiC), silicon nitride (Si
3N
4), titanium carbide (TiC), wolfram varbide (WC) and tungsten-cobalt carbide alloy (WC-Co) have been used to make die.But above-mentioned various carbide ceramics hardness are very high, are difficult to be processed into needed profile, particularly high precision aspheric surface shape.And superhard alloy uses for some time also high temperature oxidation may take place afterwards except that being difficult to processing.
So, be die core substrate with carbide or superhard alloy, the composite structure mould core that its surface is formed with other material coating or coating becomes new developing direction, typical composite structure mould core such as United States Patent (USP) the 4th, 685, No. 948 and the 5th, 202, No. 156.
United States Patent (USP) the 4th, 685, No. 948 a kind of composite structure mould cores that are used for direct compression molding opticglass product of announcement.It adopts high-intensity superhard alloy (Super-hard Alloy), carbide ceramics or sintering metal (Cermet) as die core substrate, and be formed with iridium (Ir) thin film layer in the mold pressing surface of die, or the alloy firm layer of Ir and platinum (Pt), rhenium (Re), osmium (Os), rhodium (Rh) or ruthenium (Ru), or Ru thin film layer, or the alloy firm layer of Ru and Pt, Re, Os, Rh.
United States Patent (USP) the 5th, 202 discloses the method that a kind of preparation is used for the composite structure mould core of opticglass product No. 156.It adopts high-intensity superhard alloy, carbide ceramics or sintering metal as die core substrate, and forms one deck diamond-film-like (DLC, Diamond Like Carbon) in the mold pressing surface of die.Wei Zhongshan, Zuo Dunwen be at " aviation accurate manufacturing technology " Vol.40, No.1, and 20-23 (Feb.2004) has introduced the preparation method and the application of diamond-film-like in " preparation of diamond-film-like and application " literary composition.
Yet, the rete of above-mentioned composite structure mould core wear-resisting (Wear Resistance) performance is still undesirable, after duration of service is long, be worn away easily or cracking (Crack) occur, peel off (Chip Off), tiny crack situations such as (Microcrack), thereby influence the precision of die and the quality of compression molding glassy product, work-ing life is not long.
In view of this, provide a kind of wear resisting property good, work-ing life, long die was necessary in fact.
[summary of the invention]
Not good for die wear resisting property in the solution prior art, the problem that work-ing life is long the object of the present invention is to provide a kind of wear resisting property good, die that work-ing life is long and preparation method thereof.
For realizing purpose of the present invention, the invention provides a kind of die with wearing layer, it comprises:
Mold matrix, its have one with desire the corresponding mold pressing surface of molded product; An and wearing layer that is covered in this mold pressing surface; Wherein this wearing layer thickness is in 20 nanometer to 200 nanometer range.
Described mold matrix is by pottery, sintering metal or the manufacturing of superhard alloy material, comprises SiC, Si, Si
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Described wearing layer material comprises silicon carbide (SiC), wolfram varbide (WC), silicon nitride (Si
3N
4), titanium nitride (TiN), boron carbon nitrogen (BCN), platinum (Pt), iridium (Ir), osmium (Os), rhenium (Re), rhodium (Rh), palladium (Pd).
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
For realizing another object of the present invention, the invention provides a kind of method for preparation of die kernel with wearing layer, it comprises:
One mold matrix is provided, its have one with desire the corresponding mold pressing surface of molded product;
Depositing a layer thickness by sputtering method or chemical Vapor deposition process (CVD, Chemical Vapor Deposition) on described mold pressing surface is wearing layer in 20 nanometer to 200 nanometer range.
Described mold matrix is by pottery, sintering metal or the manufacturing of superhard alloy material, comprises SiC, Si, Si
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Described sputtering method comprises bias voltage reactive sputtering (Bias Reactive Sputtering), radio-frequency sputtering (RFSputtering, Radio Frequency Sputtering) and cosputtering (Co-sputtering).
Described wearing layer material comprises silicon carbide (SiC), wolfram varbide (WC), silicon nitride (Si
3N
4), titanium nitride (TiN), boron carbon nitrogen (BCN), platinum (Pt), iridium (Ir), osmium (Os), rhenium (Re), rhodium (Rh), palladium (Pd).
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
The present invention can also further carry out rapid thermal annealing (RTA, Rapid ThermalAnnealing) to described wearing layer.
Compared with prior art, the present invention forms the nano level wearing layer on the mold matrix mold pressing surface of high rigidity, utilize the good characteristics of nano level wearing layer wear resisting property, make die of the present invention when mold pressing, be difficult to be worn away or cracking (Crack) occur, peel off (Chip Off), tiny crack situations such as (Microcrack), can increase repetition pressing mold number of times, thereby significantly prolong die work-ing life.
[description of drawings]
Fig. 1 is the synoptic diagram that the present invention is used for the die of mold pressing aspherics glassy product;
Fig. 2 is that the present invention passes through the synoptic diagram that the bias voltage reactive sputtering forms wearing layer;
Fig. 3 is the present invention forms wearing layer by radio-frequency sputtering a synoptic diagram;
Fig. 4 is the enlarged diagram of matching network among Fig. 3;
Fig. 5 is the present invention forms wearing layer by cosputtering a synoptic diagram.
[embodiment]
The present invention is described in further detail below in conjunction with accompanying drawing.
See also Fig. 1, the invention provides a kind of die 10 that is used for mold pressing aspherics glassy product, the wearing layer 103 that it comprises a mold matrix 101 and is formed on mold matrix 101 mold pressing surface 102.Described wearing layer 103 thickness are in 20 nanometer to 200 nanometer range.
Described mold matrix 101 can be that main raw gets through the sintering manufacturing: SiC, Si, Si by following pottery, sintering metal or superhard alloy
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Described wearing layer material 103 comprises SiC, WC, Si
3N
4, TiN, BCN, Pt, Ir, Os, Re, Rh, and Pd.
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
The mold pressing surface 102 of described mold matrix 101 needs corresponding with the shape of the aspherics glassy product for the treatment of mold pressing, i.e. aspheric surface shape.
Certainly, the present invention not only can be used for the die of mold pressing aspherics glassy product, also can be applicable to the die of the molded product of other different shapes, different purposes.
The present invention also is provided at the method that deposits wearing layer on the described mold matrix by sputtering method or chemical Vapor deposition process.
See also Fig. 2, first method is to deposit wearing layer 103 by the bias voltage reactive sputtering on mold matrix 101.
One vacuum system (Vacuum System) 100 forms rough vacuum by mechanical pump 150 earlier, opens high vacuum valve 160 then, and makes base pressure (Base Pressure) less than 5 * 10 by turbo-pump 140
-7Holder (Torr).To place the mold matrix 101 of described vacuum system 100 inside to link to each other by matching network (Matching Network) 110 with injection frequency power 120; One target 106 links to each other with direct supply 130 by negative electrode 107, makes between mold matrix 101 and the target 106 and forms electric field.
By first flow controller (MFC, Mass Flow Rate Controller) 170, second flow director 180 control argon gas (Ar) and nitrogen (N
2) flow; Between mold matrix 101 and target 106, form electricity slurry district (Plasma) 105, positive ion and electronics that ionization produces bombard target 106 at a high speed, atom or molecule on the target 106 are sputtered out, and deposition one layer thickness is the wearing layer 103 in 20 nanometer to 200 nanometer range on mold matrix 101.
Described mold matrix 101 can be that main raw gets through the sintering manufacturing: SiC, Si, Si by following pottery, sintering metal or superhard alloy
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Described wearing layer 103 comprises Si
3N
4, TiN, BCN, Pt, Ir, Os, Re, Rh, and Pd layer.
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
In the described bias sputtering bias voltage scope of mold matrix 101 be-40V～-100V so that described wearing layer 103 has stress (Compressive Stress), make it that adhesion and mechanical property be arranged preferably.Mold matrix 101 is not connected with bias voltage and will causes described wearing layer 103 to have tensile stress (Tensile Stress), makes described wearing layer 103 poor adherence and occur cracking or tiny crack easily.
The present invention can also further carry out rapid thermal annealing to described wearing layer 103, and the scope of annealing temperature is 250～500 ℃, and should be higher than depositing temperature.Thereby reduce described wearing layer 103 unrelieved stresss (ResidualStress), and reduce grain size (Grain Size), reduce surfaceness (Surface Roughness).
Second method provided by the invention also is to deposit wearing layer by the bias voltage reactive sputtering on mold matrix, wherein, except that with power supply that the mold matrix negative bias is connected, each condition is all identical with first method.In present method, described mold matrix directly is connected with the direct supply negative bias.
See also Fig. 3 and Fig. 4, the third method of the present invention is to deposit wearing layer by radio-frequency sputtering on mold matrix 201.
One vacuum system 200, it mainly comprises the target 206 that a mold matrix 201 and links to each other with radio-frequency power supply 220 by negative electrode 207 and matching network 210.
By first flow controller 270, second flow director, 280 control sputter gas flows; Between mold matrix 201 and target 206, form electricity slurry district 205, positive ion and electronics that ionization produces bombard target 206 at a high speed, atom or molecule on the target 206 are sputtered out, and deposition one layer thickness is the wearing layer in 20 nanometer to 200 nanometer range on mold matrix 201.
Described mold matrix 201 can be that main raw gets through the sintering manufacturing: SiC, Si, Si by following pottery, sintering metal or superhard alloy
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Described wearing layer comprises SiC and WC layer.
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
Among Fig. 4 vacuum system 200 is represented with load (Load) form; Comprise electric capacity 211 and inductor block 212 in the matching network 210, make that the forward output rating (Forward Power) of radio-frequency power supply 220 can be modulated and maximization, so that oppositely output rating (Reflecting Power) minimizes.
The present invention can also further carry out rapid thermal annealing to described wearing layer, and the scope of annealing temperature is 250～500 ℃, and should be higher than depositing temperature.Thereby reduce described wearing layer unrelieved stress, and reduce grain size, reduce surfaceness.
See also Fig. 5, the 4th kind of method of the present invention is to deposit wearing layer by cosputtering on mold matrix 301.
One vacuum system 300, it mainly comprises a mold matrix 301, a target 306 and a target 308.Form high vacuum by mechanical pump 350 and turbo-pump 340; And described mold matrix 301 linked to each other with radio-frequency power supply 320 by matching network 310, described target 306 links to each other with radio-frequency power supply 321 by negative electrode 307, described target 308 links to each other with direct supply 330 by negative electrode 309, makes between mold matrix 301 and target 306 and 308 and forms electric field.
By first flow controller 370, second flow director, 380 control argon gas (Ar) and nitrogen (N
2) flow; Between mold matrix 301 and target 306 and 308, form electricity slurry district 305, and make mold matrix 301 with 15 to 100rpm (Rotation Per Minute, rev/min) rotating speed rotation, positive ion and electronics that ionization produces bombard target 306 and 308 at a high speed, atom or molecule on target 306 and 308 are sputtered out respectively, and deposition one layer thickness is the wear-resisting mixed membranous layer in 20 nanometer to 200 nanometer range on mold matrix 301.
Described mold matrix 301 can be that main raw gets through the sintering manufacturing: SiC, Si, Si by following pottery, sintering metal or superhard alloy
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Described wearing layer comprises TiN and Si
3N
4Mixed membranous layer or with Pt, Ir, Os, Re, Rh, and Pd in the mixed membranous layer that forms of any two kinds of materials.
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
The present invention can also further carry out rapid thermal annealing to described wearing layer, and the scope of annealing temperature is 250～500 ℃, and should be higher than depositing temperature.Thereby reduce described wearing layer unrelieved stress, and reduce grain size, reduce surfaceness.
In addition to the above methods, the present invention can be TiN or Si in 20 nanometer to 200 nanometer range by CVD method deposit thickness on mold matrix also
3N
4Wearing layer.Its reaction formula is as follows:
3SiH
4+4NH
3→Si
3N
4+12H
2
6TiCl
4+8NH
3→6TiN+N
2+24HCl
Described mold matrix can be that main raw gets through the sintering manufacturing: SiC, Si, Si by following pottery, sintering metal or superhard alloy
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co.
Preferably, described wearing layer thickness is in 50 nanometer to 100 nanometer range.
The present invention can also further carry out rapid thermal annealing to described wearing layer, and the scope of annealing temperature is 250～500 ℃, and should be higher than depositing temperature.Thereby reduce described wearing layer unrelieved stress, and reduce grain size, reduce surfaceness.
Die of the present invention, its mold matrix has high rigidity, the advantage of high mechanical properties, the pressure that produces in the time of can bearing hot press moulding and stress. The mold pressing surface of mold matrix is covered by the nanoscale wearing layer, and described wearing layer is that the material by high-fracture toughness (Fracture Toughness) forms these material fracture toughness values KICScope be 2～16Mpa.m05, maximum mould temperature can reach more than 600 ℃, and the highest withstand temperature is 1200～1400 ℃, and the scope of the maximum briquetting pressure of pressing mold is 10KN～30KN. Described wearing layer can further reduce residual stress behind rapid thermal annealing, reduce crystal grain and reduce surface roughness, both can strengthen the mechanical strength on die surface, and the precision of mold pressing surface is improved. Utilize the good characteristics of nanoscale wearing layer anti-wear performance, so that die of the present invention is when mold pressing, be difficult to be worn away or cracking (Crack) occur, peel off the situations such as (Chip Off), micro-crack (Microcrack), repeat pressing mold 10,000 to 1,000,000 time, still can keep the high accuracy of mold pressing surface, avoid affecting the optical glass quality, thereby significantly prolong the service life of die. In sum, the die with wearing layer of the present invention has high mechanical properties, the good characteristics of anti-wear performance.
Claims (16)
1. die with wearing layer, it comprises:
One mold matrix, it has a mold pressing surface;
An and wearing layer that is covered in described mold matrix mold pressing surface;
It is characterized in that described wearing layer thickness is in 20 nanometer to 200 nanometer range.
2. the die with wearing layer as claimed in claim 1 is characterized in that, described mold matrix is by SiC, Si, Si
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co make.
3. the die with wearing layer as claimed in claim 2 is characterized in that, described wearing layer material comprises silicon carbide, wolfram varbide, silicon nitride, titanium nitride, boron carbon nitrogen, platinum, iridium, osmium, rhenium, rhodium, palladium.
4. as any described die in the claim 1 to 3, it is characterized in that described wearing layer thickness is in 50 nanometer to 100 nanometer range with wearing layer.
5. as any described die in the claim 1 to 3, it is characterized in that the mold pressing surface of described die is an aspheric surface with wearing layer.
6. method for preparation of die kernel with wearing layer, it comprises:
One mold matrix is provided, and it has a mold pressing surface;
On described mold pressing surface, deposit one deck wearing layer by sputtering method or chemical Vapor deposition process;
It is characterized in that described wearing layer thickness is in 20 nanometer to 200 nanometer range.
7. the method for preparation of die kernel with wearing layer as claimed in claim 6 is characterized in that, described mold matrix is by SiC, Si, Si
3N
4, ZrO
2, Al
2O
3, TiN, TiO
2, TiC, B
4C, WC, W or WC-Co make.
8. the method for preparation of die kernel with wearing layer as claimed in claim 7 is characterized in that described sputtering method comprises bias voltage reactive sputtering, radio-frequency sputtering and cosputtering.
9. the method for preparation of die kernel with wearing layer as claimed in claim 8 is characterized in that, when described sputtering method was the bias voltage reactive sputtering, the bias voltage scope of described mold matrix was-and 40V～-100V.
10. the method for preparation of die kernel with wearing layer as claimed in claim 9 is characterized in that, described wearing layer comprises silicon nitride layer, titanium nitride layer, boron carbonitride layer, platinum layer, iridium layer, osmium layer, rhenium layer, rhodium layer and palladium layer.
11. the method for preparation of die kernel with wearing layer as claimed in claim 8 is characterized in that, when described sputtering method was radio-frequency sputtering, described wearing layer comprised silicon carbide layer and carbide layers.
12. the method for preparation of die kernel with wearing layer as claimed in claim 8, it is characterized in that, when described sputtering method is cosputtering, described wearing layer comprise titanium nitride and silicon nitride mixolimnion or with Pt, Ir, Os, Re, Rh, and Pd in the mixolimnion of any two kinds of material formation.
13. the method for preparation of die kernel with wearing layer as claimed in claim 7 is characterized in that, when described chemical Vapor deposition process deposited, described wearing layer comprised titanium nitride layer or silicon nitride layer.
14., it is characterized in that described wearing layer thickness is in 50 nanometer to 100 nanometer range as any described method for preparation of die kernel in the claim 6 to 13 with wearing layer.
15. as any described method for preparation of die kernel in the claim 6 to 13, it is characterized in that with wearing layer, also be included in described wearing layer deposition after, this wearing layer of quick thermal annealing process.
16. the method for preparation of die kernel with wearing layer as claimed in claim 15 is characterized in that, the scope of the annealing temperature of described quick thermal annealing process is 250 ℃ to 500 ℃, and is higher than depositing temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2004100521575A CN1769226B (en) | 2004-11-06 | 2004-11-06 | Wearing layer-possessing mould core and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2004100521575A CN1769226B (en) | 2004-11-06 | 2004-11-06 | Wearing layer-possessing mould core and its preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1769226A CN1769226A (en) | 2006-05-10 |
| CN1769226B true CN1769226B (en) | 2010-04-28 |
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|---|---|---|---|
| CN2004100521575A Expired - Fee Related CN1769226B (en) | 2004-11-06 | 2004-11-06 | Wearing layer-possessing mould core and its preparation method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603209A (en) * | 2011-01-25 | 2012-07-25 | 鸿富锦精密工业（深圳）有限公司 | Coated glass and preparation method thereof |
| CN102643034A (en) * | 2011-02-21 | 2012-08-22 | 鸿富锦精密工业（深圳）有限公司 | Functional glass and preparation method thereof |
| CN104843972B (en) * | 2015-03-26 | 2018-04-27 | 苏州含光微纳科技有限公司 | A kind of new core rod for being used for optical lens processing and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5538528A (en) * | 1993-01-07 | 1996-07-23 | Matsushita Electric Industrial Co., Ltd. | Glass optical element press-molding die having a tantalum containing alloy surface layer |
| CN1524813A (en) * | 2003-01-24 | 2004-09-01 | 奥林巴斯株式会社 | Mould for forming optical elements and the optical elements |
| CN1541958A (en) * | 2003-04-28 | 2004-11-03 | 鸿富锦精密工业（深圳）有限公司 | Die assembly for producing optical glass products and manufacturing method thereof |
-
2004
- 2004-11-06 CN CN2004100521575A patent/CN1769226B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5538528A (en) * | 1993-01-07 | 1996-07-23 | Matsushita Electric Industrial Co., Ltd. | Glass optical element press-molding die having a tantalum containing alloy surface layer |
| CN1524813A (en) * | 2003-01-24 | 2004-09-01 | 奥林巴斯株式会社 | Mould for forming optical elements and the optical elements |
| CN1541958A (en) * | 2003-04-28 | 2004-11-03 | 鸿富锦精密工业（深圳）有限公司 | Die assembly for producing optical glass products and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JP特开平11-79757A 1999.03.23 |
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| CN1769226A (en) | 2006-05-10 |
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