CN101945828A - Mold regenerating method - Google Patents

Mold regenerating method Download PDF

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Publication number
CN101945828A
CN101945828A CN2009801055742A CN200980105574A CN101945828A CN 101945828 A CN101945828 A CN 101945828A CN 2009801055742 A CN2009801055742 A CN 2009801055742A CN 200980105574 A CN200980105574 A CN 200980105574A CN 101945828 A CN101945828 A CN 101945828A
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Prior art keywords
tectum
forming mould
oxidation
zone
forming
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Inventor
速水俊一
福本直之
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Konica Minolta Opto Inc
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Konica Minolta Opto Inc
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • C03B11/06—Construction of plunger or mould
    • C03B11/08—Construction of plunger or mould for making solid articles, e.g. lenses
    • C03B11/084—Construction of plunger or mould for making solid articles, e.g. lenses material composition or material properties of press dies therefor
    • C03B11/086—Construction of plunger or mould for making solid articles, e.g. lenses material composition or material properties of press dies therefor of coated dies
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2215/00—Press-moulding glass
    • C03B2215/02—Press-mould materials
    • C03B2215/03—Press-mould materials defined by material properties or parameters, e.g. relative CTE of mould parts
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2215/00—Press-moulding glass
    • C03B2215/02—Press-mould materials
    • C03B2215/08—Coated press-mould dies
    • C03B2215/10—Die base materials
    • C03B2215/12—Ceramics or cermets, e.g. cemented WC, Al2O3 or TiC
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2215/00—Press-moulding glass
    • C03B2215/02—Press-mould materials
    • C03B2215/08—Coated press-mould dies
    • C03B2215/14—Die top coat materials, e.g. materials for the glass-contacting layers
    • C03B2215/16—Metals or alloys, e.g. Ni-P, Ni-B, amorphous metals

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

Provided is a method for regenerating molds for press molding of glass material, which molds have a mold base material and at least one coating layer provided on said mold base material. After removing at least a portion of the coating layer (coating layer removal process) and then removing an oxide layer formed during the coating layer removal process (oxide layer removal process), the coating layer is re-formed (coating layer formation process).

Description

The forming mould renovation process
Technical field
The present invention relates to the renovation process of forming mould, this forming mould is used for extrusion forming glass material, makes the glass forming body that is used for optical element etc.
Background technology
Make the method for glass forming bodies such as optical element as extrusion forming glass material, known two kinds of methods that the heated-die pressing process and the drop method of forming are arranged again.Heated-die pressing process is with forming mould the glass preform of making in advance that institute decides quality and shape that has to be carried out the heating and pressurizing moulding again, and this method is because of not needing equipment such as glass melting furnace, so be widely adopted.
The drop method of forming is that the melten glass that drips on the forming mould that is heated to institute's fixed temperature (counterdie) drips, and the melten glass that drips with forming mould pressurization, moulding drips, and obtains glass forming body.This method can be dripped direct manufacturing glass forming body from melten glass because do not need the heating and cooling repeatedly of forming mould, so can shorten the needed time of moulding greatly 1 time, is attracted attention.
As the forming mould of making glass forming body with aforesaid method,, be widely used in and form tectal forming mould on the precision machined mould base material from the protection of molding surface and the viewpoints such as release property of raising glass.
Processing this forming mould generally needs a large amount of time and labors, and mould is very expensive according to material itself, so require mould to have high-durability.But tectum is through extrusion forming is impaired easily repeatedly, defective such as take place that part is peeled off easily, so, the forming mould that does not obtain having abundant weather resistance so far as yet.
To this, there are discussion and motion that forming mould method of life (please refer to for example patent documentation 1,2) is regenerated, prolonged to impaired tectum.The method of record in the patent documentation 1 is that to establish between mould base material and upper layer with chromium be the middle layer of main component, removes this middle layer with chromium solvability treatment solution.In addition, the method for record is to establish the middle layer between mould base material and upper layer in the patent documentation 2, by the irradiation of ionic fluid, removes the topmost in scalping and middle layer, dissolves then and removes the middle layer.
In addition, in the drop method of forming, because melten glass drips the conflict counterdie and on the following face (face that contacts with counterdie) airtrapping takes place sometimes.In order to prevent this phenomenon, have and a kind of the method for asperitiesization (Rmax:0.05 μ m～0.2 μ m) is carried out by motion (please refer to patent documentation 3) in the counterdie surface.Also has a kind of counterdie by motion, wherein be at the tectum of the last formation of the basal surface of asperitiesization (Ra:0.005 μ m～0.05 μ m), contain useful fixed treatment solution in this tectum and carry out the dissolved dissolving layer, thus when preventing airtrapping by making dissolving layer dissolving, can easily regenerate (please refer to patent documentation 4).
Patent documentation 1: the spy opens flat 1-192733 communique
Patent documentation 2: the spy opens the 2001-130918 communique
Patent documentation 3: the spy opens flat 3-137031 communique
Patent documentation 4: the spy opens the 2005-272187 communique
Summary of the invention
The problem that the invention desire solves
But, described in patent documentation 1,2,4,, compare deterioration before tectal closely connected property and the regeneration in dissolving, when forming tectum, regeneration forming mould after removing tectum once more, the weather resistance that can not get requiring has problems.And the regeneration of forming mould will cause the reduction of the closely connected property of more significant tectum repeatedly.Therefore, the forming mould that is difficult to regenerate, use repeatedly, this becomes the big reason that hinders the glass forming body cost to reduce.
In addition, be used for the situation of the forming mould of the drop method of forming, described in patent documentation 3,4, under the situation of surperficial asperitiesization, the impaired surfaceness that makes that extrusion forming causes changes (roughness reduction), then with compare the lost of life usually.Therefore, must carry out the regeneration of forming mould continually, the closely connected property of the tectum reduction that regeneration causes especially becomes big problem.
The present invention is in view of above-mentioned technical problem, and purpose is to provide a kind of renovation process of forming mould, and wherein, the reduction of the closely connected property of tectum that causes of preventing to regenerate can be regenerated repeatedly.
With the means that solve problem
In order to solve above-mentioned problem, the present invention has following feature.
(1) a kind of forming mould renovation process, described forming mould comprise the mould base material and be located at least 1 layer tectum on this mould base material, is used for extrusion forming glass material, and the forming mould renovation process is characterised in that,
Have: tectum is removed operation, removes described tectal at least a portion; Tectum forms operation, forms the described tectum that has been removed again;
Also have zone of oxidation and remove operation, before described tectum forms operation, remove the zone of oxidation that forms on the surface after having removed described tectal at least a portion.
(2) the forming mould renovation process of record in above-mentioned (1) is characterized in that described glass material is that the melten glass that drips drips, and also has asperities chemical industry preface, after described tectum forms operation, by corroding described cover surface asperitiesization.
(3) the forming mould renovation process of record in above-mentioned (1) or (2) is characterized in that described mould base material is made of silicon carbide.
(4) the forming mould renovation process of record in above-mentioned (3) is characterized in that, described mould base material is to form silicon carbide layer with the CVD method on the sintered compact of silicon carbide.
(5) the forming mould renovation process of putting down in writing in any one of above-mentioned (1) to (4) is characterized in that, it is the operation of removing described zone of oxidation with the physics gimmick that described zone of oxidation is removed operation.
(6) the forming mould renovation process of putting down in writing in any one of above-mentioned (1) to (4) is characterized in that, it is the operation of removing described zone of oxidation with chemical gimmick that described zone of oxidation is removed operation.
(7) the forming mould renovation process of record in above-mentioned (6) is characterized in that it is the operation of corroding described zone of oxidation with fluorine class corrosive fluid that described zone of oxidation is removed operation.
(8) the forming mould renovation process of putting down in writing in any one of above-mentioned (1) to (7) is characterized in that, described tectum contains at least a kind of element of chromium, aluminium, titanium.
(9) the forming mould renovation process of putting down in writing in any one of above-mentioned (1) to (8) is characterized in that, it is to adopt the corrosion process of acidic solution that described tectum is removed operation.
(10) the forming mould renovation process of putting down in writing in any one of above-mentioned (1) to (9), it is characterized in that, have asperities chemical industry preface, after described tectum forms operation, making the described tectal surface that forms again is that arithmetic mean roughness (Ra) is 0.01 μ m～0.2 μ m, and the average length (RSm) of coarse curve element is that 0.5 μ m carry out asperitiesization followingly.
The effect of invention
According to the present invention, before forming tectal operation again, the operation of removing the zone of oxidation that forms when removing tectum is arranged, thus can prevent the reduction of the tectal closely connected property that forms again, can the repeated regeneration forming mould.
Description of drawings
Fig. 1: the forming mould renovation process flow process signal of the 1st embodiment.
Fig. 2: the forming mould state model synoptic diagram (sectional view) of the 1st each operation of embodiment.
Fig. 3: the forming mould renovation process flow process signal of the 2nd embodiment.
Fig. 4: the forming mould state model synoptic diagram (sectional view) of the 2nd each operation of embodiment.
Nomenclature
10,20 forming moulds
11 mould base materials
12 tectums
13 zone of oxidation
14 tectal surfaces
15 molding surface
The S101 tectum is removed operation
The S102 zone of oxidation is removed operation
The S103 tectum forms operation
S104 asperities chemical industry preface
Embodiment
1 to accompanying drawing 4 with reference to the accompanying drawings, describes embodiments of the present invention in detail.
[the 1st embodiment]
Fig. 1 is the forming mould renovation process flow process signal of the present invention's the 1st embodiment.Fig. 2 is the forming mould state model synoptic diagram (sectional view) of each operation.
Forming mould
Forming mould 10 before Fig. 2 (a) expression regeneration.Forming mould 10 comprises mould base material 11 and at least 1 layer of tectum 12 that is located on the mould base material 11.On the tectum 12, because extrusion forming impaired repeatedly, exist part to peel off and defective (not diagram) such as crack.
On mould base material 11, establish the molding surface 15 of the shape that formalizes with known precision sizing method.The shape of molding surface 15 does not have particular restriction, can be corresponding with the glass forming body of making, get different shapes such as sphere, aspheric surface, cylindrical surface.Can be that convex surface also can be a concave surface.
The forming mould that the material of mould base material 11 can be used from known extrusion forming glass material is with the material, suitably select to use according to condition.Can enumerate for example various refractory alloy (stainless steel etc.), be the superhard material of main component, various pottery (silicon carbide, silicon nitride etc.), carbon-containing composite material etc. with the wolfram varbide.
Wherein especially silicon carbide (SiC) is thermotolerance and the excellent especially material of weather resistance, but the closely connected property reduction of regeneration back tectum 12 is obvious, so the forming mould that mould base material 11 is made of SiC was difficult to use repeatedly by regeneration in the past.According to the present invention, even mould base material 11 is the forming moulds that are made of SiC, the closely connected property reduction of tectum 12 after also can preventing from effectively to regenerate can be used repeatedly by regeneration.Especially on the SiC sintered compact, form the forming mould of SiC layer, have and to suppress material cost and be lower advantage by the CVD method.
Tectum 12 improves viewpoint such as release property and is provided with for protection mould base material 11 molding surface 15 with to glass, can use various materials formations such as metal, nitride, oxide compound.Wherein, the material that especially preferably contains at least a element of chromium, aluminium, titanium.The film that contains these elements not only easily film forming, have the advantage that can easily remove by corrosion, also have the feature of surface oxidation, the stabile oxide skin of formation by heating in atmosphere.The standard free energy of formation of chromium, aluminium, titanium oxide (standard Gibbs energy of formation) is all little, very stable, so also be not easy the bigger advantage of reacting even have to contact with the high-temperature fusion glass drop.
As the material of at least a element that contains chromium, aluminium, titanium, can enumerate for example chromium metal, metallic aluminium, metal titanium, chromium nitride, aluminium nitride, titanium nitride, chromic oxide, aluminum oxide, titanium oxide etc.
Tectum 12 also can have the multilayered structure more than 2 layers as long as establish 1 layer at least.The thickness of tectum 12 does not have particular restriction, but the function of too thin call protection molding surface 15 grades is insufficient, so usually preferably more than 0.05 μ m.Otherwise it is big that the too thick words film thickness distribution of tectum 12 becomes, and is easy to generate the out of shape and film of molding surface 15 shapes sometimes and defective such as peels off.Therefore, the preferred 0.05 μ m of tectum 12 thickness～5 μ m, especially preferred 0.1 μ m～1 μ m.When tectum 12 had multilayered structure, preferred aggregate thickness was in above-mentioned scope.
Tectum is removed operation S101
It is the operation of removing at least a portion of tectum 12 from impaired forming mould 10 that tectum is removed operation S101.Fig. 2 (b) expression is removed operation S101 has removed tectum 12 from forming mould 10 state through tectum.
Removing of tectum 12 can be undertaken by corrosion.Corrosion can be the wet corrosion that adopts corrosive fluid, also can be to adopt isoionic dry corrosion.
Wet corrosion is the method that reactive etching liquid contact tectum 12, dissolving tectum 12 are removed, and does not need expensive equipment, can also easily remove tectum 12.Can be impregnated into tectum 12 in the corrosion liquid bath, also can on tectum 12, supply with quantitative corrosive fluid.It can also be the method for spraying shape corrosive fluid.
Corrosive fluid can suitably be selected known corrosive fluid according to the material of tectum 12.When tectum 12 was aluminium, various acidic solutions etc. had sale as aluminium with the corrosive fluid that can preferably adopt.When tectum 12 is titanium, with the corrosive fluid that can preferably adopt sale is arranged also as titanium.Can enumerate for example is the corrosive fluid of main component with reductive acids such as hydrochloric acid, sulfuric acid.
When tectum 12 is the situation of chromium, same, with the corrosive fluid that can preferably adopt sale is arranged also as chromium.Can enumerate acidic solution that for example contains ceric ammonium nitrate etc.In addition, also can adopt the basic solution that contains the Tripotassium iron hexacyanide and potassium hydroxide.
And adopt isoionic dry etching method, be in vacuum chamber, to import corrosion gas, make the ion and the atomic group that produce plasma, generate carry out removing of tectum 12 by plasma by high frequency etc.Sometimes be called as plasma etching, reactive ion corrosion (RIE) etc.Because do not produce waste liquid, little to carrying capacity of environment, also have foreign matter less and the reproducibility excellence of handling etc., so be preferable methods to the pollution on surface.
Corrosion gas can be rare gas elementes such as Ar, also can adopt the reactive high gas of halogens such as containing F, Cl, Br.Gas (the CF for example that wherein especially contains halogens such as F, Cl, Br 4, SF 6, CHF 3, Cl 2, BCl 3, HBr etc.) reactive high with tectum 12, can handle with the short period of time.Can also adopt above-mentioned gas and と O 2, N 2Deng mixed gas.The device of dry corrosion can suitably be selected to use from known device such as parallel plate-type, bucket (cylinder) type, magnetron-type, ECR type, does not have particular restriction.
Tectum is removed and be there is no need to spread all over whole molding surface 15 ground among the operation S101 and remove tectum 12, as long as remove the tectum 12 in molding surface 15 part zones (for example during glass ware forming and the zone of glass contact).In addition, can remove all tectums 12 by corrosion when tectum 12 has multilayered structure, also can stay in the tectum 12 near mould base material 11 which floor and only remove the face side layer.
The present inventor finds, removes formation zone of oxidation 13 on the surface after the tectum 12 in order to remove tectum 12 with corrosion, and the existence of this zone of oxidation 13 is the reasons that cause the closely connected property reduction of the tectum 12 after the regeneration.
When for example mould base material 11 was SiC, because tectum crevice corrosion liquid etc. when removing operation S101, mould base material 11 surfaces formed by SiO 2Zone of oxidation 13 Deng the oxide compound formation.The tectum 12 closely connected property that form on this zone of oxidation 13 are low, peel off easily during extrusion forming etc.Especially when tectum 12 is metallic substance and the bonding property of oxide compound bad, closely connected property significantly reduces.And repeated regeneration causes zone of oxidation 13 thickness thickenings, and the closely connected property of tectum 12 is more and more lower.
Among the present invention,,, remove the operation (zone of oxidation is removed operation S102) of the zone of oxidation 13 that when removing tectum 12, forms forming tectum 12 operations (tectum forms operation S103) more before in order to prevent the reduction of above-mentioned tectum 12 closely connected property.
Zone of oxidation is removed operation S102
It is as follows that zone of oxidation is removed operation S102: before tectum forms operation, remove the zone of oxidation 13 that forms on the surface after at least a portion of removing tectum 12.Fig. 2 (c) expression is removed operation S102 by zone of oxidation and has been removed zone of oxidation 13 mould base material 11 states afterwards.
The method of removing zone of oxidation 13 has physics gimmick and chemical gimmick.The physics gimmick has methods such as very aerial ion bombardment, grinding, and wherein, from can be easily and remove the viewpoint of zone of oxidation 13 definitely, grinding be effective.Grind material from preventing molding surface 15 shapes viewpoint out of shape, compare preferred employing alumina with diamond.When for example mould base material 11 is SiC, be that alumina about 1 μ m serves as to grind material, carry out grinding in tens of seconds to several minutes, can prevent that thus molding surface 15 shapes are out of shape and definitely remove zone of oxidation 13 with size of particles.
And corrosion is the effective chemical gimmick.Corrode to have and be difficult for causing molding surface 15 shapes advantage out of shape.When for example mould base material 11 is SiC, carry out corrosion in several minutes, can remove zone of oxidation 13 definitely thus with diluted hf.Corrosive fluid is not limited to diluted hf, removes can preferably adopting of zone of oxidation 13 as long as can not damage mould base material 11 ground.Here said zone of oxidation 13 is the thin layers about tens of nm～100 nm, and some also can corrosion rate slowly.In addition, fluorine class corrosive fluids such as diluted hf are not because corrode the SiC of mould base material 11, so, have and remove the zone of oxidation 13 (SiO that form with homogeneous film thickness 2Film) and the almost constant advantage of optical surface shape.
Tectum forms operation S103
It is as follows that tectum forms operation S103: be formed on tectum again and remove the tectum 12 that operation S101 removes, forming mould 10 is regenerated.Fig. 2 (d) is illustrated in the state that the surface of having removed after the zone of oxidation 13 has formed tectum 12 again.Because remove in above-mentioned zone of oxidation and to have removed zone of oxidation 13 among the operation S102, form tectum 12 so can not reduce closely connected property ground.
The formation method of tectum 12 can suitably be selected to use from known film without limits.Can enumerate for example vacuum plating gas method, the method for splashing, CDVD method etc.Wherein, the method for splashing is the big tectum 12 of the closely connected power of film forming easily, so preferred.
In addition, in order to improve the closely connected property of tectum 12, preferably the zone of oxidation before forming tectum 12 is removed and is fully removed adherent grinding material and corrosive fluid etc. among the operation S102.
[the 2nd embodiment]
Subsequent with reference to Fig. 3, Fig. 4, the renovation process of the forming mould of the surperficial asperitiesization that is used for the drop method of forming is explained.Fig. 3 is the flow process signal of present embodiment forming mould renovation process.Fig. 4 is the forming mould state model synoptic diagram (sectional view) of each operation in the present embodiment.
Forming mould 20 in Fig. 4 (a) expression present embodiment before the regeneration.Forming mould 20 is identical with the situation of the 1st embodiment, comprises mould base material 11 and at least 1 layer the tectum 12 that is located on the mould base material 11.The surface 14 of tectum 12 by asperities turn to fixed surfaceness, still, extrusion forming causes that roughness reduces repeatedly, surfaceness is compared with appropriate scope and is diminished.Sometimes part also occurring peels off and defectives such as crack.The material of mould base material 11 and tectum 12 is identical with the situation of above-mentioned forming mould 10.
As mentioned above, in the drop method of forming, by with surperficial asperities change forming mould as accepting the counterdie that melten glass drips, can prevent that residual air accumulates on glass forming body.
In addition, in the drop method of forming, because be that the glass of molten state contacts with forming mould, so forming mould and glass are easy to generate adhesion.But, by adopt surperficial asperities change forming mould, can prevent adhesion with glass.This effect with surperficial asperities change forming mould during as the situation of counterdie and as the situation of patrix, can both obtain equally.
Tectum shown in Fig. 3 is removed operation S101, zone of oxidation removes operation S102 and tectum formation operation S103 is identical with the situation of the 1st embodiment shown in Fig. 1.Fig. 4 (b) expression is removed operation S101 has removed tectum 12 from forming mould 20 state by tectum, Fig. 4 (c) expression is removed the state that operation S102 has removed the mould base material 11 after the zone of oxidation 13 by zone of oxidation, and Fig. 4 (d) is illustrated in the state that the surface of having removed after the zone of oxidation 13 has formed tectum 12 again.
Asperities chemical industry preface S104
S104 is as follows for asperities chemical industry preface: by corrosion asperitiesization carry out in tectum 12 surfaces 14 that form again.The asperitiesization on Fig. 4 (e) expression carrying out tectum 12 surfaces 14, the forming mould 20 of regeneration completion status.
Especially preferably the arithmetic average roughness (Ra) that makes tectum 12 surfaces 14 is that the average length (RSm) of 0.01 μ m～0.2 μ m and roughness curve key element carry out asperitiesization below 0.5 μ m.Average length (RSm) by making arithmetic average roughness (Ra) and roughness curve key element can prevent airtrapping and adhesion effectively in above-mentioned scope.
The average length (RSm) of arithmetic average roughness (Ra) and roughness curve key element is the roughness parameter that defines among the JIS B 0601:2001.The mensuration of above-mentioned parameter adopts carries out as the mensuration machine of the sort of spatial image resolving power of AFM (atomic force microscope) below 0.1 μ.General contact pin type roughness is measured machine because the radius-of-curvature of contact pilotage tip is big to number μ m, so not preferred.
Corroding method is not particularly limited, can suitably selects to implement from removing in the identical method of the method that illustrated the operation S101 with tectum.When tectum 12 contained the chromium element, following method (1) or (2) were because of not needing expensive main equipment, can carrying out the processing of excellent in uniformity with low cost effectively, so preferred.
(1) employing contains the wet corrosion of the acidic solution of ceric ammonium nitrate
(2) employing contains the wet corrosion of the basic solution of the Tripotassium iron hexacyanide and potassium hydroxide
As corrosive fluid, also can be when only adopting common acidic solution such as sulfuric acid, nitric acid, perchloric acid to tectum 12 asperitiesization.But above-mentioned by adopting (1) contains ceric ammonium nitrate (Ce (NH 4) 2(NO 3) 6) acidic solution, can be evenly and form fine concavo-convex in short time on tectum 12 surfaces 14 that contain the chromium element.As long as contain ceric ammonium nitrate, also can be the solution that contains multiple acid such as nitric acid, perchloric acid.The concentration of ceric ammonium nitrate can be so that to the suitably selection of the institute processing speed of hoping ground, common preferred 5 quality %～50 quality %.
Also can be when in addition, only adopting common basic solution such as sodium hydroxide, potassium hydroxide to tectum 12 asperitiesization as corrosive fluid.But above-mentioned by adopting (2) contain the basic solution of the Tripotassium iron hexacyanide and potassium hydroxide, can be evenly and form fine concavo-convex in short time on tectum 12 surfaces 14 that contain the chromium element.As the basic solution that contains the Tripotassium iron hexacyanide and potassium hydroxide, can adopt for example mixed solution of the Tripotassium iron hexacyanide, potassium hydroxide and pure water.And can include other composition in the scope that does not influence effect of the present invention.As for the ratio of the Tripotassium iron hexacyanide and potassium hydroxide, preferably for the Tripotassium iron hexacyanide 1 mass parts, potassium hydroxide is 0.2～5 mass parts.The combined amount of pure water does not have particular restriction, can make reach the processing speed of hoping ground suitably select.
In addition, in order to carry out stabile processing, preferably keep certain treatment chamber air themperature and illumination, counterdie temperature, handle conditions such as number, corrosive fluid temperature, amount, concentration.On the contrary, by changing these conditions, can suitably adjust the formed concavo-convex degree of depth and cycle.
[embodiment]
Embodiment 1,2
The method according to this invention is carried out the regeneration of forming mould repeatedly, makes glass forming body with the drop method of forming simultaneously, has confirmed the weather resistance (tectal closely connected property) of forming mould.
Forming mould 10 shown in Fig. 2 (embodiment 1) is as patrix, and the forming mould 20 shown in Fig. 4 (embodiment 20) is as counterdie.Two mould base materials 11 all are SiC (forming the SiC layer with the CVD method on the SiC sintered compact), and tectum 12 is individual layer chromium (metals).
Forming mould 10 (patrix) is according to flow process shown in Fig. 1, and per 2000 injections are regenerated.Forming mould 20 (counterdie) is according to flow process shown in Fig. 3, and per 1000 injections are regenerated.Tectum is removed the chromium corrosive fluid that contains ceric ammonium nitrate that operation S101 adopts sale, and (Na カ ラ イ テ ス Network Co., Ltd. makes, and ECR-2), removes tectum 12 by corrosion.Zone of oxidation is removed zone of oxidation 13 among the operation S102 and is removed with fluoric acid and carry out.Tectum 12 among the tectum formation operation S103 forms and carries out with the method for splashing.
By wet corrosion forming mould 20 is carried out the asperitiesization on tectum 12 surfaces 14 then.Corrosive fluid uses Tripotassium iron hexacyanide 100g, potassium hydroxide 100g and pure water 1L blended mixed solution (basic solution).Arithmetic average roughness after the asperitiesization (Ra) is 0.1 μ m, and the average length (RSm) of roughness curve key element is 0.25 μ m.(Digital Instruments company makes the average length (RSm) of arithmetic average roughness (Ra) and roughness curve key element, D3100) measures with AFM.
Carry out forming mould regeneration with above-mentioned condition, add up to the moulding of 8000 injections simultaneously.The regeneration times of forming mould 10 (patrix) is 3 times, and the regeneration times of forming mould 20 (counterdie) is 7 times.Glass material employing Tg is 480 ℃ a phosphoric acid class glass.Counterdie was heated to 500 ℃, patrix and is heated to 450 ℃ when forming mould used.Melten glass drips quality and is about 190mg, and the loading during pressurization is 1800N.
After the moulding,, confirmed and represented that not the defective that film is peeled off takes place tectum 12, does not have the reduction of the closely connected property of tectum 12 even find to regenerate repeatedly yet with the resulting glass ware forming of 50 times observation by light microscope surface.In table 1 (forming mould 10) and table 2 (forming mould 20), show the result.
[table 1]
Figure BPA00001205418900111
[table 2]
Figure BPA00001205418900121
[comparative example 1,2]
Different with embodiment 1,2, do not carry out zone of oxidation and remove the regeneration that operation S 102 just carries out forming mould, carried out adding up to the moulding of 8000 injections.In addition other regeneration condition is identical with embodiment 1,2 with condition of molding.
After the moulding, on the glass ware forming surface, confirmed expression tectum 12 defective that film is peeled off has taken place.Therefore, investigated to the frequency injection that film is peeled off takes place by regeneration times.The result shows in table 1 and table 2 together.
Shown in table 1, table 2, each regeneration, the patrix counterdie all is to the frequency injection minimizing that film is peeled off takes place.Therefore, confirmed and do not carried out zone of oxidation and remove operation S102 ground and carry out forming mould when regeneration, repeated regeneration can cause tectum 12 closely connected property reductions.

Claims (10)

1. forming mould renovation process, described forming mould comprise the mould base material and be located at least 1 layer tectum on this mould base material, is used for extrusion forming glass material, and the forming mould renovation process is characterised in that,
Have: tectum is removed operation, removes described tectal at least a portion; Tectum forms operation, forms the described tectum that has been removed again;
Also have zone of oxidation and remove operation, before described tectum forms operation, remove the zone of oxidation that forms on the surface after having removed described tectal at least a portion.
2. as the forming mould renovation process of record in the claim 1, it is characterized in that described glass material is that the melten glass that drips drips, and has asperities chemical industry preface, after described tectum forms operation, by corroding to described cover surface asperitiesization.
3. as the forming mould renovation process of record in claim 1 or 2, it is characterized in that described mould base material is made of silicon carbide.
4. as the forming mould renovation process of record in the claim 3, it is characterized in that described mould base material is to form silicon carbide layer with the CVD method on the sintered compact of silicon carbide.
5. the forming mould renovation process as putting down in writing in any one of claim 1 to 4 is characterized in that it is the operation of removing described zone of oxidation with the physics gimmick that described zone of oxidation is removed operation.
6. the forming mould renovation process as putting down in writing in any one of claim 1 to 4 is characterized in that it is the operation of removing described zone of oxidation with chemical gimmick that described zone of oxidation is removed operation.
7. as the forming mould renovation process of record in the claim 6, it is characterized in that it is the operation of corroding described zone of oxidation with fluorine class corrosive fluid that described zone of oxidation is removed operation.
8. the forming mould renovation process as putting down in writing in any one of claim 1 to 7 is characterized in that described tectum contains at least a kind of element of chromium, aluminium, titanium.
9. the forming mould renovation process as putting down in writing in any one of claim 1 to 8 is characterized in that, it is to adopt the corrosion process of acidic solution that described tectum is removed operation.
10. the forming mould renovation process as putting down in writing in any one of claim 1 to 9, it is characterized in that, have asperities chemical industry preface, after described tectum formed operation, making the described tectal surface that forms again was that arithmetic mean roughness (Ra) is that the average length (RSm) of 0.01 μ m～0.2 μ m, coarse curve element is that asperitiesization carry out to it in the following ground of 0.5 μ m.
CN2009801055742A 2008-02-21 2009-02-17 Mold regenerating method Pending CN101945828A (en)

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JP2008039812 2008-02-21
JP2008-039812 2008-02-21
PCT/JP2009/052660 WO2009104585A1 (en) 2008-02-21 2009-02-17 Mold regenerating method

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Publication number Priority date Publication date Assignee Title
ES2517740B1 (en) * 2013-04-29 2015-08-05 Construcciones Y Reparaciones Mecánicas Sivó, S. L. Procedure for the recovery of molds for manufacturing glass parts and containers

Citations (5)

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Publication number Priority date Publication date Assignee Title
JPH0238330A (en) * 1988-07-29 1990-02-07 Hoya Corp Regeneration of glass-forming tool
JPH06345447A (en) * 1993-06-03 1994-12-20 Canon Inc Method for regenerating mold for forming optical element
JP2005272187A (en) * 2004-03-23 2005-10-06 Konica Minolta Opto Inc Mold for optical element and regenerating method thereof
JP2006089327A (en) * 2004-09-24 2006-04-06 Hoya Corp Method of manufacturing optical device and mold for forming optical device
JP2006111504A (en) * 2004-10-18 2006-04-27 Pentax Corp Method for regenerating mold for forming optical glass

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0238330A (en) * 1988-07-29 1990-02-07 Hoya Corp Regeneration of glass-forming tool
JPH06345447A (en) * 1993-06-03 1994-12-20 Canon Inc Method for regenerating mold for forming optical element
JP2005272187A (en) * 2004-03-23 2005-10-06 Konica Minolta Opto Inc Mold for optical element and regenerating method thereof
JP2006089327A (en) * 2004-09-24 2006-04-06 Hoya Corp Method of manufacturing optical device and mold for forming optical device
JP2006111504A (en) * 2004-10-18 2006-04-27 Pentax Corp Method for regenerating mold for forming optical glass

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WO2009104585A1 (en) 2009-08-27

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