CN100493912C - Substrate for ink jet head, ink jet head utilizing the same and producing method therefor - Google Patents
Substrate for ink jet head, ink jet head utilizing the same and producing method therefor Download PDFInfo
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- CN100493912C CN100493912C CNB200380107491XA CN200380107491A CN100493912C CN 100493912 C CN100493912 C CN 100493912C CN B200380107491X A CNB200380107491X A CN B200380107491XA CN 200380107491 A CN200380107491 A CN 200380107491A CN 100493912 C CN100493912 C CN 100493912C
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Abstract
For improving adhesion between a protective layer having a portion coming into contact with ink in a substrate for an ink jet head, and a resin layer thereby ensuring reliability in quality over a prolonged period, the invention provides a substrate for an ink jet head including a heat-generating resistor constituting a heat generating portion, an electrode wiring electrically connected with the heat-generating resistor and an upper protective layer provided on the heat-generating resistor and the electrode wiring across an insulating protective layer, wherein after forming an upper protective layer in which a Ta layer is laminated on a layer formed by a TaCr alloy, said Ta layer is selectively patterned and selectively removed so that the liquid flow path member is formed in a portion where the layer formed by said TaCr alloy is exposed by said removing.
Description
Technical field
The present invention relates to be used for by being discharged to such as the functional liquid of printing ink on the recording medium that comprises paper, plastic sheet, cloth, article etc. and the used substrate of the ink gun of record or printable character, symbol or image; Use the ink gun and the manufacture method thereof of this substrate.
Background technology
A kind of conventional structure that is used for the ink gun of ink mist recording comprises a plurality of outlets, the ink flow passage that links to each other with these outlets and a plurality of electrothermal conversioning element that can produce the heat energy that is used for ink-jet.Described electrothermal conversioning element provides the electrode of electric energy to constitute by giving birth to thermal resistor with the thermal resistor of making a living, and this electrothermal conversioning element scribbles insulation film to guarantee the insulation between each electrothermal conversioning element.Each ink flow passage links to each other with common liquid chamber at its place, end relative with outlet, and described common liquid chamber stores the printing ink of supplying with from the ink box as printing ink storage container parts.The printing ink that supplies to common liquid chamber leads to each ink flow passage so that printing ink forms meniscus near outlet.In this state, electrothermal conversioning element is selectively driven to produce heat energy, and described heat energy is used to cause bubble fast at the lip-deep printing ink of thermo-contact, so that discharge printing ink under by the pressure that described state variation caused.
Between expulsive stage, the heat effect of ink gun part is exposed under the higher temperature by the heating of giving birth to thermal resistor at printing ink, simultaneously, and mainly is subjected to because the immixture of the chemical action of cavitation shock that the bubble of printing ink forms and contraction causes and printing ink.
Therefore, heat effect part has usually and is used to protect electrothermal conversioning element not to be subjected to the upper protective layer of the chemical action of described cavitation shock and printing ink.
Tradition, the Ta film that can stand the chemical action of cavitation shock and printing ink largely is formed to such an extent that have the thickness of 0.2 to 0.5 μ m, thereby can increase the service life of ink gun, obtains reliability simultaneously.
In addition, in described heat effect part, can cause a kind of like this phenomenon; promptly; be included in look material in the printing ink, additive etc. owing to be heated under the high temperature, thereby thereby they on molecular level, decompose to form and be difficult to dissolved substances, described material physically is absorbed on the upper protective layer.This phenomenon is known as fouling (kogation).Organic and the inorganic substances that are difficult to dissolve are absorbed in by this way and can cause on the upper protective layer conducting to the inhomogeneous heat of printing ink from giving birth to thermal resistor, thereby cause unsettled bubble to produce.Therefore, common use is not easy to the outstanding Ta film of fouling.
Below with reference to Fig. 8, with the generation of bubble and the pattern of disappearance in the printing ink that is described in the heat effect part.
In Fig. 8, curve (a) shows at driving voltage V
Op=1.3 * V
Th(V
ThThe threshold voltage that produces for the bubble of printing ink), driving frequency is set to 6kHz and pulse width is set under the situation of 5 μ s, the moment when voltage is applied in living thermal resistor begins the surface temperature change in time of upper protective layer.In addition, curve (b) shows the growth state of the bubble that the moment when voltage is applied in living thermal resistor in a similar manner begins to produce.Shown in curve (a); begin the rising of temperature from the moment that voltage applies, and delayed slightly arrives temperature rise peak value (this is slightly to arrive upper protective layer evening owing to come from the heat of living thermal resistor) in the predetermined pulse time, afterwards; because thermal diffusion, temperature mainly reduces.On the other hand, shown in curve (b), when the temperature when upper protective layer reaches about 300 ℃, begin the growth of bubble, and reach maximum bubblement afterwards, and disappear.In actual ink gun, carry out aforesaid operations in the mode that repeats.Along with the bubble in the printing ink produces, the surface of upper protective layer is elevated to for example about 600 ℃, and how this explanation comprises the heat effect of high temperature in ink mist recording.
Therefore, require to have outstanding membrane property at aspects such as hear resistance, mechanical property, chemical stability, non-oxidizability, alkali resistances with the contacted upper protective layer of printing ink.As the material that is used in the upper protective layer aspect; except that the above-mentioned Ta film of mentioning, noble metal, high-melting-point transition metal, the alloy of these metals, nitride, boride, silicide or carbide, the non-crystalline silicon etc. of these metals in addition known in the prior art.For example, described among the Japanese patent application laid-open publication number No.2001-105596, upper protective layer has been formed on the living thermal resistor, and used by composition formula Ta via insulating barrier
αFe
βNi
γCr
δThe amorphous alloy of expression (wherein satisfy 10at.%≤α≤30at.%, alpha+beta〉80at.%, α＜β, δ〉γ and alpha+beta+δ+γ=100at.%) make upper protective layer; wherein the contact surface of itself and printing ink comprises the oxide of its component substances, and has proposed a kind of more reliable record head of long life that has.
Yet, in recent years, for in higher-quality document image and the ink jet recording device such as more high performance increases in demand such as high-speed records, and in order to satisfy these demands, require the ink performance of enhancing, for example, in order to obtain that the high-quality document image has proposed the requirement of improved painted characteristic and weather resistance and in order to obtain the requirement that high-speed record has proposed to prevent bleeding (obscuring between the different colours printing ink).Therefore, made the trial of in printing ink, adding various compositions.The kind of printing ink has had variation, except that black, yellow, magenta and cyan, also has the light color inks such as less dense.Described printing ink causes a kind of like this corrosion phenomenon, that is, or even thinking stably on the Ta film as upper protective layer, owing to the thermal chemical reaction with printing ink causes corrosion.Use therein to comprise such as divalent metal salt such as calcium and magnesium or constitute under the situation of printing ink of composition of chelate, can occur above-mentioned phenomenon more significantly.
On the other hand, because higher corrosion resistance makes the surface can damage hardly, thereby the velocity of discharge of printing ink is lowered or becomes unstable, and therefore aforesaid have the corrosive upper protective layer of improved anti-printing ink and be easier to produce fouling.Probably seldom produce fouling in traditional Ta film, this is because the Ta film produces corrosion and fouling on a certain equilibrium level, thereby thereby the surface of Ta film can be suppressed the deposition of fouling product by described corrosive wear.
In addition, in order in ink mist recording, to realize higher writing speed, drive with shorter pulse execution thereby need further to increase driving frequency.In described driving with short pulse more because in the heat effect part of ink gun, repeat at short notice to heat, the program of bubble generation, bubble collapse and cooling, therefore with conventional ADS driving in compare, in shorter time, produce bigger thermal stress.In addition; in the driving of short pulse more; to come from the time shorter that bubble in the printing ink produces and the cavitation shock of bubble shrinkage concentrates on the diaphragm of top, so need exist in the upper protective layer that mechanical shock characteristic aspect is particularly splendid than conventional ADS driving.
In order to form ink gun with the ink gun substrate that described upper protective layer is housed; disclosed in Japanese patent application laid-open publication number No.H6-286149; used a kind of like this method; promptly; use soluble resin to form ink flow path by the lithoprinting forming technique; afterwards with the covering and the described patterns that hardens such as epoxy resin, and when being cut into piece, removes described substrate described soluble resin.
Disclosed in Japanese patent application laid-open publication number No.2002-113870; also can realize higher durability and the reliability of Geng Gao in the following manner; described mode promptly; upper protective layer is configured has two-layerly, use high anti-ink corrosion amorphous state Ta film to use and lowly produce the Ta film of fouling as the upper strata as lower floor.
Yet; make printing ink discharge element elongation (to 0.5 inch or bigger) so that realize under the situation of higher writing speed or use comprise the diversified printing ink of additive so that improve printing ink light resistance on the recording medium or the situation of anti-gaseousness under; owing to the difference in the linear expansion coefficient of described parts and owing to the stress in the resin bed of the wall that constitutes flow path or outlet has produced strain; and the influence of newtype printing ink on the interface, thereby cause constituting the phenomenon of peeling off between the covering resin layer of wall of flow path or outlet and the upper protective layer on the heater substrate.In addition; even under organic adhesion promoter layer is arranged on situation on the upper protective layer; also can cause the peeling off at the interface between organic adhesion promoter layer and the upper protective layer; thereby make the printing ink health to substrate and cause the corrosion of connecting up, thereby hindered record or reliability satisfied in the long term.
Summary of the invention
What an object of the present invention is to improve the substrate that is used for ink gun has and the upper protective layer of the contacted part of printing ink and the adhesion between the resin bed, thereby the substrate that can guarantee the ink gun of reliability and be used for described ink gun in over a long time is provided.
Another object of the present invention provides a kind of substrate that is used for ink gun, has the ink gun of described substrate; with and manufacture method; even wherein at the point that has used the more fine definition that is used for document image or be used under the situation of longer recording element of higher writing speed; thereby perhaps using diversified printing ink can obtain under the more highdensity situation of record head, described substrate also has improved adhesion between upper protective layer and resin bed.
Another object of the present invention provides a kind of even also can realize the structure of the upper protective layer of high durability and high reliability for highly corrosive printing ink, thus be provided for the substrate of ink gun and the ink gun of long life with and manufacture method.
Another object of the present invention provides a kind of substrate that is used for ink gun; comprise being formed with and be used to produce in order to the substrate of the living thermal resistor of the energy of discharging printing ink, the electrode wiring that is electrically connected with described living thermal resistor; and be located at the top of described living thermal resistor and described electrode wiring and comprise the upper protective layer of TaCr alloy; it is characterized in that described upper protective layer has the structure and the described resin structure that are formed from a resin and is fixed on the described upper protective layer on the part at an upper portion thereof.
Another object of the present invention provides a kind of ink gun; comprise the outlet that is used to discharge liquid; communicate with described outlet and have and be used for applying flow path in order to the part of the heat energy of discharging described liquid to described liquid; be used to produce the living thermal resistor of described heat energy; the electrode wiring that is electrically connected with described living thermal resistor; and be located at the top of described living thermal resistor and described electrode wiring and comprise the upper protective layer of TaCr alloy; it is characterized in that described upper protective layer has the structure and the described resin structure that are formed from a resin and is fixed on the described upper protective layer on the part at an upper portion thereof.
Another object of the present invention provides a kind of manufacture method of ink gun; described ink gun comprises on substrate: constitute the living thermal resistor of heat unit branch, the electrode wiring that is electrically connected with described living thermal resistor; be located on described living thermal resistor and the described electrode wiring and have upper protective layer with the contacted contact surface of printing ink, and be formed on flow path element on the described substrate by resin bed.Described manufacture method comprises: form Ta layer wherein and be laminated on by the step of the upper protective layer on the formed layer of TaCr alloy, optionally described Ta layer formed pattern and optionally remove the step of described Ta layer, form the step of flow path element in the part that exposes formed layer of TaCr alloy by described removal step.
Another object of the present invention provide a kind of substrate that is used for ink gun, ink gun with and manufacture method; wherein have outstanding adherence between upper protective layer and the resin bed and can under pinpoint accuracy, form the pattern of flow path; thereby provide the ink gun of high reliability; in addition even the peeling off of element that under ink gun is lengthened to 0.5 inch or higher situation, also can not cause constituting flow path, thus in long-time, guarantee high reliability.
Another object of the present invention provide a kind of substrate that is used for ink gun, ink gun with and manufacture method; wherein said ink gun can form the pattern of flow path by the outstanding adherence between upper protective layer and the resin bed under pinpoint accuracy; thereby even form or be used to realize at the point of the more fine definition that is used to realize document image and also can guarantee high reliability under the situation of high-speed driving of higher writing speed.
Description of drawings
Fig. 1 is the partial cross section figure that is used for the substrate of ink gun of the present invention;
Fig. 2 A, 2B, 2C and 2D show the view that is used for being used for forming on the substrate of ink gun of the present invention the method for discharging element;
Fig. 3 A, 3B, 3C, 3D and 3E show the view that is used for being used for forming on the substrate of ink gun of the present invention the another kind of method of discharging element;
Fig. 4 shows the view of the film forming device of the layer that is used to form the substrate that is used for ink gun of the present invention;
Fig. 5 is a schematic diagram, shows the structure that ink gun of the present invention is applied to ink jet recording device wherein;
Fig. 6 shows the part ink gun that is used for being used for forming on the substrate of ink gun of the present invention another embodiment that discharges element;
Fig. 7 is the schematic partial cross section figure of Fig. 6; And
Fig. 8 is a chart, shows at voltage and applies temperature change and the bubble generation state of back in upper protective layer.
The specific embodiment
Fig. 1 is schematic partial cross section figure, shows the ink gun that structure of the present invention is suitable for.
In Fig. 1; show silicon substrate 101; the heat accumulation layer of making by heat oxide film 102; for example by the SiO film; the interlayer film 103 of heat accumulation is made and be used for to SiN film etc.; give birth to thermal resistor layer 104; by such as Al; Al-Si; and the metal wiring layer 105 that constitutes of metal material such as Al-Cu; for example by the SiO film; the protective layer 106 of insulating barrier is made and be used as to SiN film etc.; being located at being used on the protective layer 106 protects electrothermal conversioning element not to be subjected to the chemistry relevant with giving birth to heat that thermal resistor produced and the upper protective layer 107 of physical impact; and heat effect part 108; in this heat effect part 108, the heat that living thermal resistor produced of giving birth to thermal resistor layer 104 is transferred on the printing ink.
Heat effect part in the ink gun is exposed under the high temperature owing to giving birth to the heat that produces in the thermal resistor, and the bubble that is mainly come from the printing ink produces or the cavitation shock of bubble shrinkage afterwards and the chemical action of printing ink.Therefore, upper protective layer 107 is arranged on this heat effect and partly goes up so that protect electrothermal conversioning element not to be subjected to the chemical action of described cavitation shock and printing ink.On upper protective layer 107, the element 109 that is used to form flow path has formed the discharge element that comprises outlet 110.
Fig. 2 A shows the method for discharging element that is used to form to 2D.
On the ink gun substrate 200 identical, apply anticorrosive additive material by spin-coating method, as the soluble solids layer 201 that is used for finally constituting ink flow path with the ink gun substrate 100 shown in Fig. 1.The anticorrosive additive material of being made by PMIPK (poly-methyl isopropenyl ketone, polymethylisopropheyl ketone) is configured as the shape of ink flow path as the negative interaction resist and by use photolithography method with it.Subsequently, form coating resin layer 203 so that form the wall of flow path or outlet.Before forming this coating resin layer 203, can compatibly carry out the processing of silane coupling connection and wait to improve adhesion.By the known coating process of suitable selection, coating resin layer 203 can be coated on the ink gun substrate 200 of the pattern that holds ink flow path.Afterwards, by the rear surface formation ink supply port 206 from ink gun substrate 200 such as anisotropic etch method, blasting method or anisortopicpiston engraving method.Better, can form ink supply port 206 by the chemical anisotropic etch method of using tetramethyl azanol (TMAH), NaOH or KOH etc.In order to remove soluble solids layer 201, carry out by far ultraviolet and expose fully, develop and drying subsequently.
To as shown in the 3E, forming upper protective layer 107 (Ta as Fig. 3 A
100-xCr
x) afterwards, can below the nozzle composed component, form organic adhesion and promote film 307.Select the polyetheramides resin to promote film 307 as organic adhesion.Because outstanding anti-alkaline corrosivity, for such as the adherence of the satisfaction of the organic film of silicon and the advantage that can be used as the anti-printing ink diaphragm of ink jet print head, therefore described resin is particularly preferred.Afterwards as Fig. 3 A to as shown in the 3E, carry out photoetching process to form pattern.Can realize described formation pattern by dry etching similar methods with common organic film.More particularly, the etching by oxygen gas plasma realizes described formation pattern as mask can to utilize the positive interaction resist.
In the following description, to 3E, be described in upper protective layer 107 (Ta with reference to Fig. 3 A
100-xCr
x) formation after, be used to form the method that organic adhesion promotes film 307.On ink gun substrate 300, apply anticorrosive additive material so that form the final soluble solids layer 301 that constitutes ink flow path by spin-coating method.The anticorrosive additive material of being made by PMIPK (poly-methyl isopropenyl ketone, polymethylisopropheyl ketone) is configured as the shape of ink flow path as the negative interaction resist and by the photolithography method with it.
Subsequently, form coating resin layer 303 so that form the wall of flow path or outlet.Before forming this coating resin layer 303, can compatibly carry out the processing of silane coupling connection and wait to improve adhesion.By the known coating process of suitable selection, coating resin layer 303 can be applied the substrate that is used for ink-jet of the pattern that is formed with ink flow path thereon.Be that coating resin layer 303 forms pattern by the photolithography method afterwards.Afterwards, by the rear surface formation ink supply port 306 from substrate such as anisotropic etch method, blasting method or anisortopicpiston engraving method.Better, can form ink supply port 306 by the chemical anisotropic etch method of using tetramethyl azanol (TMAH), NaOH or KOH etc.In order to remove soluble solids layer 301, carry out by far ultraviolet and expose fully, develop and drying subsequently.
The substrate that uses cast-cutting saw etc. will carry the nozzle segment that forms to 2D and 3A to the step described in the 3E by Fig. 2 A cuts into chip, and described chip receives and is electrically connected so that drive and give birth to thermal resistor, also supplies element with printing ink to be connected, thereby finishes ink gun.
Requirement will have such as at outstanding membrane properties in aspect such as thermal resistance, mechanical property, chemical stability, non-oxidizability, alkali resistances with the contacted upper protective layer of printing ink; and for the adherence of organic adhesion promoter layer and nozzle composed component, and constitute by Ta and Cr.Preferably by Ta
100-xCr
xConstitute, wherein x 〉=12at.%.
From 50nm to 500nm, select the film thickness of upper protective layer 107 in the scope of (preferably from 100nm to 300nm).And this upper protective layer has compression at least, preferably is no more than 1.0 * 10
10Dyn/cm
2Can make upper protective layer 107 by the whole bag of tricks, but can use radio frequency (RF) power supply or direct current (DC) power supply to make usually by magnetron sputtering system.
Fig. 4 shows the sputtering equipment that is used to form upper protective layer 107.In Fig. 4, show Ta target and Cr target 4001, flat target 4002, be used to control film formed flashboard 4011 on the substrate, substrate holder 4003, substrate 4004, the power supply that is connected with substrate holder 4003 with target 4001.In Fig. 4, also show the external heater 4008 that provides in the mode that forms the periphery wall of chamber 4009 around film.External heater 4008 is used to regulate the environment temperature that film forms chamber 4009.The interior heater 4005 that is used to regulate underlayer temperature is arranged on the rear surface of substrate holder 4003.Best and external heater 4008 combined realization substrate temperatures are controlled.
Carrying out the film that uses Fig. 4 equipment as follows forms.At first, use vavuum pump 4007 that film is formed chamber 4009 and be evacuated to 1 * 10
-5To 1 * 10
-6Pa.Next, introducing hole 4010 via gas is incorporated into argon gas in the film formation chamber 4009 by the mass flow controller (not shown).In this operation, so regulate interior heater 4005 and external heater 4008 so that underlayer temperature and environment temperature become predetermined temperature.Then, power is provided to target 4001 so that form the sputter discharge from power supply 4006, and regulates flashboard 4011 so that form film on substrate 4004.
In the present invention, two types target promptly, can form by utilizing Ta target and Cr target and carrying out film from two power supplys that are attached thereto respectively to the synchronous sputtering method of the binary of wherein supplying power.In this case, can regulate the power that is fed to each target independently.Perhaps, also can be by preparing multiple alloys target that its composition regulated in advance and the sputter of carrying out single target or multiple alloys target are had desired constituents with formation by the while sputter film.
Aforesaid, when forming upper protective layer 107, obtain strong film adhesiveness to 300 ℃ by substrate being heated to up to 100 ℃.In addition, the sputtering method formation film that has than the particle of kinetic energy can be formed, strong film adhesiveness can be obtained by foregoing.
(be no more than 1.0 * 10 by making film have compression at least
10Dyn/cm
2), can obtain strong film adhesiveness equally.Can regulate described membrane stress by suitably setting the heating-up temperature that is incorporated into the flow velocity of the argon gas in the film forming device, the power that puts on target or substrate.
Fig. 5 shows the external view of the ink-jet apparatus that the present invention is suitable for.This ink-jet apparatus is old-fashioned, but the present invention is more effective when being applied to nearest ink-jet apparatus.
In the ink-jet apparatus shown in Fig. 5, record head 2200 is installed on the balladeur train 2120 that engages with the helicla flute 2121 of guide spiro rod 2104, described guide spiro rod 2104 rotates with the rotation forward or backwards of CD-ROM drive motor 2101 by driving force transmission gear 2102 and 2103, and moves back and forth with balladeur train 2120 along guide rail 2119 along direction a and b by the power of CD-ROM drive motor 2101.The pressboard 2105 that is used for being transmitted in the record-paper P on the pressing plate 2106 by recording medium supply equipment (not shown) is pressed in pressing plate 2106 along the moving direction of balladeur train 2120 with record-paper.
The bar 2117 that is used to begin to be used to aspirate recovery operation moves along with moving of the cam 2118 that engages with balladeur train 2120, thereby by control the driving force of CD-ROM drive motor 2102 such as the transmitting device of clutch.Be used for sending signal to the living hot cell 2110 that is located at record head 2200 and be used for controlling the record control unit (not shown) that said mechanism drives and be set at the recording equipment main body.
The ink jet recording device 2100 of Gou Chenging is by making record head 2200 move back and forth executive logging on the whole width that is transported to the record-paper P on the pressing plate 2106 by the recording medium supply equipment as mentioned above, and because record head 2200 is to make with the method described in aforementioned, therefore described equipment can be realized high-precision high-speed record.
Hereinafter, describe the present invention with reference to the formation example and the use of upper protective layer 107 in detail by the example of the ink gun of this upper protective layer.Yet the present invention is not limited to described example.
When the Ta-Cr film that will be used for upper protective layer 107 is formed on the silicon wafer, use equipment and the above-mentioned film formation method shown in Fig. 4, and estimate the characteristic of described film.Explain that in the following manner film forms the evaluation of operation and membrane property.It should be noted, do not comprise in the present invention by film form technology etc. be included in finish and do not expect element (pollutant) in the film.
[film forms operation]
At first, heat oxide film is formed on the silicon single crystal wafer, and described silicon wafer (substrate 4004) film that is set at the equipment shown in Fig. 4 forms on the substrate holder 4003 in the chamber 4009.Then, using vavuum pump 4007 that film is formed chamber 4009 is evacuated to up to 8 * 10
-6Pa.Afterwards, argon gas being incorporated into film from gas is introduced hole 4010 forms in the chamber 4009 and is following condition with its internal regulation:
[film formation condition]
Underlayer temperature: 200 ℃
Film forms the gaseous environment temperature in the chamber: 200 ℃
Film forms the gas blend pressure of chamber interior: 0.6Ppa
Then, on the heat oxide film of silicon wafer, be formed with the thick Ta of 200nm by the synchronous sputtering method of binary (wherein using variable power) that utilizes Ta target and Cr target at every kind of target
100-xCr
xFilm, thus sample 1 to 7 obtained.
On every kind of the sample 1 to 7 that is obtained, carry out constituent analysis by RBS (rutherford backscattering).The result that obtains shown in the table 1.As shown in table 1, the power that is provided to Ta target and Cr target by change can obtain the film of heterogeneity.
Table 1
[membrane stress]
Next, determine the membrane stress of each sample the substrate distortion amount before and after film forms.As a result of, along with Ta
100-xCr
xThe increase of Cr concentration in the film, membrane stress trends towards changing into tensile stress from compression, and the film adhesion trends towards reducing.Be at least compression and be no more than 1.0 * 10 by formation
10Dyn/cm
2Membrane stress, can obtain strong film adhesion.
(with the adherence of resin)
(example 1)
In order to estimate the Ta in this example simply
88Cr
12Film 107 (is meant the film of the component ratio with Ta88at.% and Cr12at.%; Represent composition hereinafter in a similar manner) and organic adhesion promote adherence between the film (polyetheramides resin) 307, carries out afterwards in pressure cooker test (PCT) and is with disbonded test.
Carry out the band disbonded test in the following manner.On the silicon wafer that carries upper protective layer 107; formed organic adhesion and promoted film (polyetheramides resin) 307, and promoted to form in the mode of 10 (vertically) * 10 (laterally)=100 a foursquare checkerboard pattern on the film 307 square of 1 * 1mm with cutter in organic adhesion with 2 μ m thickness.Pass through at 121 ℃ and 2.0265 * 10 afterwards
5In alkaline printing ink, soaked 10 hours and execution PCT under the condition of Pa (2atm.).Afterwards, adhesive tape is applied on the square in the checkerboard pattern and is stripped from, and studies among 100 squares a plurality of squares by tape stripping.As a result, although among 100 squares, observe about 15 foursquare peeling off, also obtained common gratifying result (table 2).
(comparative example 1)
Ta film in use and the example 1 after the similar methods evaluation PCT and organic adhesion promote the adherence between the film (polyetheramides resin) 307, and the result who is obtained has been shown in table 2.
As shown in table 2, promote the interface place generation between the film 307 to peel off at Ta film and organic adhesion after the PCT, obviously show the degeneration of adhesiveness.
(example 2 to 7)
Similar methods is estimated the PCT Ta of heterogeneity afterwards in use and the example 1
100-xCr
xThe adherence of film has illustrated the result who is obtained in table 2.
(comparative example 2 and 3)
Similar methods is estimated PCT adherence afterwards in use and the example 1.At Ta
20Fe
61Cr
14Ni
5(comparative example 2) and Ta
87Fe
10Cr
2Ni
1(comparative example 3) makes an appraisal, and the result who is obtained has been shown in table 2.
As from these results, understanding, be used as the Ta of top diaphragm traditionally
20Fe
61Cr
14Ni
5Film and Ta
87Fe
10Cr
2Ni
1Film can not provide sufficient adhesiveness, and this is because upper protective layer 107 and organic adhesion promote the peeling off of interface place between the film 307 to cause.
Table 2
| Film component (at.%) | Film thickness [nm] | The quantity of peeling off (after the PCT) | |
| Example 1 | Ta 88Cr 12 | 200 | 15/100 |
| Example 2 | Ta 86Cr 14 | 200 | 8/100 |
| Example 3 | Ta 82Cr 18 | 200 | 0/100 |
| Example 4 | Ta 80Cr 20 | 200 | 0/100 |
| Example 5 | Ta 70Cr 30 | 200 | 0/100 |
| Example 6 | Ta 45Cr 55 | 200 | 0/100 |
| Example 7 | Ta 27Cr 73 | 200 | 0/100 |
| Comparative example 1 | |
200 | 100/100 |
| Comparative example 2 | Ta 20Fe 61Cr 14Ni 5 | 200 | 66/100 |
| Comparative example 3 | Ta 87Fe 10Cr 2Ni 1 | 200 | 100/100 |
As previously described, after the PCT, at Ta
100-xCr
xIn the film, upper protective layer 107 and organic adhesion promote the adherence between the film 307 to trend towards step-down in the film of low Cr content, and are in the gratifying scope under x is equal to or higher than the situation of 12at.%.
Except that the aforementioned result that exists under the adhesion promoter layer situation, under the situation that does not have adhesion promoter layer, also obtained similar result, and determined regardless of existing or not having adhesion promoter layer, Ta
100-xCr
x(x 〉=12at.%) film all is effective for adherence.
[evaluation of characteristics of inkjet]
(example 8)
In this example, silicon substrate or the silicon substrate that wherein is formed with drive IC are used as the sample that is used to analyze characteristics of inkjet.In the situation of silicon substrate, form the SiO of 1.8 μ m thickness by thermal oxidation process, sputtering method or CVD method etc.
2Heat accumulation layer 102 (Fig. 1), and the silicon substrate that has had IC also in set-up procedure experience form SiO
2The process of heat accumulation layer.
Afterwards, form the SiO of 1.2 μ m thickness by sputtering method or CVD method etc.
2Interlayer dielectric 103.Afterwards, form the thick Ta of 50nm by the reactive sputtering that uses the Ta-Si target
40Si
21N
39Give birth to thermal resistor 104.Under 200 ℃ underlayer temperature, carry out this operation.Form the thick Al film of 200nm by sputtering method then as metal line 105.
Then, carry out the formation pattern to form the wherein heat effect part 108 of the removed 26 μ m of Al film * 26 μ m by the photolithography art.Then, form protective layer 106 by the plasma CVD method SiN insulation component that 300nm is thick.
Afterwards, under for the change power of Ta target and Cr target by the sputtering method Ta that 200nm is thick
88Cr
12Form upper protective layer 107.
Afterwards, be that upper protective layer 107 forms pattern by dry etching.
Subsequently, promote film (polyetheramides resin) 307 in order to improve the adherence between upper protective layer and the nozzle composed component, formed organic adhesion, thereby obtain the ink gun substrate with 2 μ m thickness.
Use described ink gun substrate with the preparation ink gun in the manufacture method shown in Fig. 3, described ink gun experiences in ink jet recording device discharges durability test.Under the pulse width of the driving frequency of 15kHz and 1 μ sec, carry out described test, and estimate 1.0 * 10 by cross-sectional view by FIB
8The wearing and tearing of upper protective layer 107 after the pulse.Driving voltage is V
Th* 1.3, V wherein
ThExpression is used for the bubble generation threshold voltage that printing ink is discharged.In addition, also use comprise about 4% have a nitric acid group divalent metal (Ca (NO
3)
24H
2O) printing ink.
As shown in table 3, can determine, although discharging up to 2.0 * 10 continuously
8Occur small wearing and tearing after the pulse, but upper protective layer still is stable, has stable discharge characteristic.
(comparative example 4)
Except that using Ta film preparation upper protective layer 107, to prepare ink gun with example 8 similar methods.As in the example 1, described ink gun experience is discharged durability test, and the result who is obtained has been shown in table 3.As shown in table 3, in comparative example 4, reaching 2.0 * 10
8Discharging before the pulse becomes no longer may.By the performed analytical proof of dismounting ink gun, corrosion has arrived living thermal resistor layer and has caused its damage.
(example 9 to 16)
Except that prepare upper protective layer 107 with composition shown in the table 3 and thickness, to prepare ink gun with example 8 similar methods.As in the example 8, described ink gun experience is discharged durability test, and the result who is obtained has been shown in table 3.
(comparative example 5 and 6)
Except that prepare upper protective layer 107 with composition shown in the table 3 and thickness, to prepare ink gun with example 8 similar methods.
As in the example 8, described ink gun experience is discharged durability test, and the result who is obtained has been shown in table 3.
As shown in table 3, Ta
20Fe
61Cr
14Ni
5(comparative example 5) shows little wear and is stable in discharging durability test.
Ta
87Fe
10Cr
2Ni
1(comparative example 6) shows approximately half wearing and tearing of film thickness.
These results represent following situation.
As what can understand, depend on Ta in the stability of resistance to wearing of discharging durability test middle and upper part protective layer 107 from the result as shown in the table 3
100-xCr
xThe composition of film, and become remarkable along with the increase of Cr content.More particularly, at Ta
100-xCr
xIn the composition of film, upper protective layer 107 stabilizer pole for wearing and tearing under the situation of x 〉=12at.%.
In addition, upper protective layer 107 preferably has 100 to 500nm film thickness.Can cause insufficient protective capability less than the film thickness of 100nm, and the film thickness that surpasses 500nm may hinder from giving birth to the effective energy conduction of thermal resistor to printing ink, thereby cause big energy to run off with respect to printing ink.
In these examples, even also can obtain outstanding durability by the film thickness of about 100nm.About membrane stress, be no more than 1.0 * 10 at least
10Dyn/cm
2Compression the strong film adhesion with outstanding durability can be provided.
As described above described in the example, by the alloy with Ta and Cr constitute upper protective layer 107, by realizing highdensity ink gun substrate, the ink-jet apparatus that has the ink gun of described substrate and described ink gun is housed forming resin (flow path forms element 109) on the upper protective layer 107 and described resin is fixed on can provide on the upper protective layer 107.
Table 3
| Film component (at.%) | Film thickness [nm] | Discharge the wearing and tearing (2.0 * 10 in the durability test 8After the pulse) | |
| Example 8 | Ta 88Cr 12 | 200 | ± |
| Example 9 | Ta 86Cr 14 | 200 | + |
| Example 10 | Ta 82Cr 18 | 200 | + |
| Example 11 | Ta 80Cr 20 | 200 | + |
| Example 12 | Ta 80Cr 20 | 100 | + |
| Example 13 | Ta 80Cr 20 | 400 | + |
| Example 14 | Ta 70Cr 30 | 200 | + |
| Example 15 | Ta 45Cr 55 | 200 | + |
| Example 16 | Ta 27Cr 73 | 200 | + |
| Comparative example 4 | |
200 | |
| Comparative example 5 | Ta 20Fe 61Cr 14Ni 5 | 200 | + |
| Comparative example 6 | Ta 87Fe 10Cr 2Ni 1 | 200 | ± |
(example 17)
In this example, upper protective layer 107 has double-decker, and, in the heat effect part, use the double-decker that constitutes by upper T a layer 111 and bottom TaCr layer 112, and below flow path forms element 109, use the single layer structure that only has lower floor 112.
More particularly, show use Ta
80Cr
20As the lower film 112 of upper protective layer 107 and use a kind of situation of Ta film as upper membrane 111.
Sputter on the insulating barrier to form by the binary of utilizing Ta target and Cr target and have Ta
80Cr
20The lower film 112 of composition and 130nm thickness.Analyze the condition that composition is determined the binary sputter in advance by the power that change is used for the Ta sputter and is used for the Cr sputter.In addition, replace the binary sputter, also can carry out and have in advance the sputter of the TaCr alloys target of principal component.
Afterwards by utilizing the Ta target to form upper strata 111 with 100nm thickness.Carrying out film in a continuous manner at same sputtering chamber forms.
Afterwards, the Ta film that constitutes upper strata 111 is peeled off the formation pattern by the normal optical carving technology by resist shaping (resist-coating, exposure and development), Ta etching and resist.
In this operation, can at random select the pattern of Ta film by photomask pattern in step of exposure.Therefore, as shown in Fig. 6 and Fig. 7, so select described pattern, that is, make and go up formation Ta film, but do not form Ta film in the place that will form flow path formation element 109 as upper strata 111 at heat unit branch (heat effect part 108).Peeling off by resist shaping (resist-coating, exposure and development), Ta etching and resist by photoetching process afterwards is that the TaCr film forms pattern.In Fig. 6; show a kind of low path element and form part 1090, described low path element forms lower pattern 1120 that part 1090 comprises that in the subregion flow path wherein forms element 109 and be laminated on upper layer pattern 1110 that organic adhesion promotes film 307, upper protective layer, bottom protective layer, gives birth to a kind of structure on thermal resistor 1080 and the electrode wiring 1050.
Carry out the etching of TaCr film by dry etching equipment, selection can obtain to have etching gas, gas pressure and the power of the selective etch ratio of following insulating protective layer.In the pattern of TaCr film forms, as shown in Figure 6, it be formed on be used to form flow path form element part 1090 below.
In addition, as shown in Figure 7, in the cross section, at the thick Ta of 230nm of the lower membrane 112 that constitutes upper protective layer 107
80Cr
20On the film, be pressed with the organic adhesion that constitutes lower liquid flow path element and flow path element 109 with described sequential layer and promote film 307, and estimate Ta in simple mode
80Cr
20Film and organic adhesion promote the adhesion between film 307 and the flow path element 109 on it.Be with disbonded test to estimate by carrying out afterwards in original state with in pressure cooker test (PCT).In this example, in order further to improve the adherence between flow path element 109 and the TaCr film, use organic adhesion to promote film 307 as lower liquid flow path element.
By at 121 ℃ and 2.0265 * 10
5In alkaline printing ink, soaked 10 hours and execution PCT under the condition of Pa (2atm.).The result who is obtained has been shown in table 4.These presentation of results Ta
80Cr
20Film has gratifying adherence.
Table 4
| Upper protective layer | Film thickness [nm] | The film that the top forms | Adherence (initially) | Adherence (behind the PCT) | The band disbonded test | |
| Example 17 | TaCr | 230 | Organic adhesion promotes film/flow path element | + | + | + |
| Comparative example 7 | Ta | 230 | Organic adhesion promotes film/flow path element | + | ± |
Ta in the lower floor 112 that constitutes upper protective layer 107
80Cr
20After the Ta film on film and formation upper strata 111 forms pattern, soluble solids layer 301 is coated on the substrate, and its exposure is constituted the shape of ink flow path with formation by spin-coating method.Can obtain the shape of ink flow path by normal masks and far ultraviolet.Lamination covering resin layer 303 afterwards is then by the exposure sources exposure and develop to form outlet 110.Subsequently, after the anisotropic etching of the silicon by having TMAH forms ink supply port 306, by directly being exposed to far ultraviolet, development and a dry part to be dissolved of removing covering resin layer 303.The substrate that uses cast-cutting saw etc. will carry the nozzle segment that forms by abovementioned steps cuts into chip, and described chip is electrically connected so that drives and give birth to thermal resistor, also realizes supplying being connected of element with printing ink, thereby finishes ink gun.
In the evaluation of the alkaline printing ink of discharging PH10, so the ink gun of preparation provides gratifying recording quality.In addition, in the situation of this ink gun, under 60 ℃, be immersed in this printing ink after 3 months, discharge at printing ink and estimate, gratifying recording quality is provided, and has not demonstrated peeling off of covering resin layer 303.
(comparative example 7)
Wherein show and only use the situation of individual layer Ta film as upper protective layer.
In this comparative example, form the thick Ta film of 230nm by the sputter of using the Ta target.
Peeling off by resist shaping (resist-coating, exposure and development), Ta etching and resist by the normal optical carving technology afterwards, is that the Ta film forms pattern.
In this operation, can at random select the pattern of Ta film by photomask pattern in step of exposure.
For simple evaluation 230nm thick Ta film and the flow path element 109 of formation lower liquid flow path element and the adherence between organic adhesion promotion film 307, carry out the band disbonded test.Be with disbonded test to estimate by carrying out afterwards in original state with in pressure cooker test (PCT).
By at 121 ℃ and 2.0265 * 10
5In alkaline printing ink, soaked 10 hours and execution PCT under the condition of Pa (2atm.).The result who is obtained has been shown in table 4.
According to these results, wherein the Ta film shows peeling off after the PCT, can confirm that adherence is at aforementioned use Ta
80Cr
20It is remarkable using in the structure of Ta film as the example 17 on upper strata 111 as the lower floor 112 of upper protective layer 107.
Afterwards, soluble solids layer 301 is coated on the substrate that carries upper protective layer 107, and its exposure is constituted the shape of ink flow path with formation by spin-coating method.Can obtain the shape of ink flow path by normal masks and far ultraviolet.Lamination covering resin layer 303 afterwards is then by the exposure sources exposure and develop to form outlet 110.Subsequently, by after with TMAH the anisotropic silicon etching being formed ink supply port 306, remove the part to be dissolved of covering resin layer 303 by directly being exposed to far ultraviolet, development and drying.The substrate that uses cast-cutting saw etc. will carry the nozzle segment that forms by abovementioned steps cuts into chip, and described chip is electrically connected so that drives and give birth to thermal resistor, also supplies element with printing ink to be connected, thereby finishes ink gun.
In the evaluation of the alkaline printing ink of discharging PH10, so the ink gun of preparation provides gratifying recording quality.Yet, under 60 ℃, being immersed in this printing ink after 3 months, this ink gun has demonstrated a undischarged part and gratifying recording quality can not be provided.In observation, observe the connection status of peeling off and confirm ink flow path of covering resin layer 303 for ink gun.
In this example; by with the heater substrate on the contacted lower floor of flow path element of top diaphragm in form the TaCr film; and by with the contacted upper strata of printing ink in form the Ta film; even at the point that has used the more fine definition that is used for document image or be used under the situation of longer recording element of higher writing speed; perhaps under the situation of using diversified printing ink; also can improve upper protective layer and constitute adherence between the resin bed of flow path; can realize more highdensity ink gun substrate and ink gun thereby provide, and the ink-jet apparatus that described ink gun is housed.
In addition; for diversified printing ink (such as demonstrating) owing to the height of fouling is discharged instable printing ink and the printing ink with highly corrosive; the double-decker of upper protective layer has been realized high durability and high reliability; thereby the ink gun of ink gun substrate and long life is provided, and the ink-jet apparatus that described ink gun is housed.
In foregoing example; a kind of like this ink jet print head has been described; wherein the discharge element such as outlet and ink flow path prepares by photoetching process; but the present invention also comprises a kind of like this structure, wherein constitutes the orifice plate of outlet or the top board of formation ink flow path and is independently formed and for example by adhesive material it is adhered on the upper protective layer.
Claims (11)
1. substrate that is used for ink gun comprises:
The living thermal resistor that on substrate, forms;
The electrode wiring that is electrically connected with described living thermal resistor; And
Is arranged on the top of described living thermal resistor and described electrode wiring and comprises Ta and the upper protective layer of the alloy of Cr, be formed with resin, and this resin is fixed in this upper protective layer on the top of this upper protective layer,
It is characterized in that described upper protective layer contains the Cr more than or equal to 12at.%.
2. according to the described substrate that is used for ink gun of claim 1, it is characterized in that the formation thing that described resin is made promotes that by organic adhesion film is fixed on the described upper protective layer.
3. according to the described substrate that is used for ink gun of claim 2, it is characterized in that described organic adhesion promotes that film is the polyetheramides resin.
4. according to each described substrate that is used for ink gun of claim 1 to 3, it is characterized in that,
The thickness of described upper protective layer is smaller or equal to 500nm more than or equal to 50nm.
5. according to each described substrate that is used for ink gun of claim 1 to 3, it is characterized in that,
The thickness of described upper protective layer is smaller or equal to 300nm more than or equal to 100nm.
6. according to each described substrate that is used for ink gun of claim 1 to 3, it is characterized in that,
Described upper protective layer has smaller or equal to 1.0 * 10
10Dyn/cm
2Compression.
7. according to the described substrate that is used for ink gun of claim 1, it is characterized in that:
The resin that forms on the described upper protective layer constitutes flow path and forms element,
Upper protective layer has double-decker part and single layer structure part, and the lower floor of described double-decker part is formed by the TaCr alloy and the upper strata is formed by Ta, and described single layer structure partly has only described lower floor,
The described lower floor of described single layer structure part and described flow path form to have organic adhesion and promotes film between the element, and the described upper strata of described double-decker part is set at least the contacted position of printing ink with the top of living thermal resistor.
8. according to the described substrate that is used for ink gun of claim 7, it is characterized in that described organic adhesion promotes that film is the polyetheramides resin.
9. ink gun comprises:
The described substrate that is used for ink gun of each of claim 1 to 7;
At the described electrical connections that is used to drive living thermal resistor that is provided with on the substrate of ink gun of being used for.
10. the preparation method of an ink gun may further comprise the steps:
On substrate, form living thermal resistor that constitutes heat unit and the electrode wiring that is electrically connected with this life thermal resistor;
It is characterized in that, further comprising the steps of:
Formation is arranged on the top of described living thermal resistor and described electrode wiring and has the step of the upper protective layer of the contact-making surface that contacts with printing ink; this upper protective layer stacked Ta layer on the layer that is formed by the TaCr alloy that contains more than or equal to the Cr of 12at.% forms
On described upper protective layer; optionally described Ta layer is formed pattern; and optionally eliminate this Ta layer; make with give birth to thermal resistor above the contacted position of printing ink form the Ta layer; but do not form the Ta layer, between the part of the layer that the described TaCr alloy that exposes by this elimination forms and described flow path element, have organic adhesion and promote film in the place that the flow path that will form the formation thing of making as resin forms element.
11. the preparation method according to the described ink gun of claim 10 is characterized in that, described organic adhesion promotes that film is the polyetheramides resin.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP380823/2002 | 2002-12-27 | ||
| JP380822/2002 | 2002-12-27 | ||
| JP2002380822 | 2002-12-27 | ||
| JP413498/2003 | 2003-12-11 |
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| Publication Number | Publication Date |
|---|---|
| CN1732086A CN1732086A (en) | 2006-02-08 |
| CN100493912C true CN100493912C (en) | 2009-06-03 |
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ID=35964217
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|---|---|---|---|
| CNB200380107491XA Expired - Fee Related CN100493912C (en) | 2002-12-27 | 2003-12-25 | Substrate for ink jet head, ink jet head utilizing the same and producing method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2024183B1 (en) * | 2006-05-02 | 2011-03-02 | Canon Kabushiki Kaisha | Ink jet head |
| JP5311975B2 (en) * | 2007-12-12 | 2013-10-09 | キヤノン株式会社 | Substrate for liquid ejection head and liquid ejection head using the same |
| JP6039411B2 (en) | 2012-12-27 | 2016-12-07 | キヤノン株式会社 | Inkjet head substrate, inkjet head, and inkjet head manufacturing method |
| JP7214409B2 (en) * | 2018-09-05 | 2023-01-30 | キヤノン株式会社 | liquid ejection head |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4866460A (en) * | 1987-02-04 | 1989-09-12 | Canon Kabushiki Kaisha | Ink jet recording head and base plate therefor |
| CN1344619A (en) * | 2000-07-31 | 2002-04-17 | 佳能株式会社 | Ink-jet head substrate, ink-jet head and its manufacture, using method of ink-jet head and ink-jet device |
| US6485131B1 (en) * | 1999-10-04 | 2002-11-26 | Canon Kabushiki Kaisha | Ink-jet head base board, ink-jet head, and ink-jet apparatus |
-
2003
- 2003-12-25 CN CNB200380107491XA patent/CN100493912C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4866460A (en) * | 1987-02-04 | 1989-09-12 | Canon Kabushiki Kaisha | Ink jet recording head and base plate therefor |
| US6485131B1 (en) * | 1999-10-04 | 2002-11-26 | Canon Kabushiki Kaisha | Ink-jet head base board, ink-jet head, and ink-jet apparatus |
| CN1344619A (en) * | 2000-07-31 | 2002-04-17 | 佳能株式会社 | Ink-jet head substrate, ink-jet head and its manufacture, using method of ink-jet head and ink-jet device |
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