WO1993009953A1 - Polycrystalline silicon-based base plate for liquid jet recording head, its manufacturing method, liquid jet recording head using the base plate, and liquid jet recording apparatus - Google Patents
Polycrystalline silicon-based base plate for liquid jet recording head, its manufacturing method, liquid jet recording head using the base plate, and liquid jet recording apparatus Download PDFInfo
- Publication number
- WO1993009953A1 WO1993009953A1 PCT/JP1992/001482 JP9201482W WO9309953A1 WO 1993009953 A1 WO1993009953 A1 WO 1993009953A1 JP 9201482 W JP9201482 W JP 9201482W WO 9309953 A1 WO9309953 A1 WO 9309953A1
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- WIPO (PCT)
- Prior art keywords
- substrate
- recording head
- jet recording
- liquid jet
- polycrystalline silicon
- Prior art date
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/16—Production of nozzles
- B41J2/1601—Production of bubble jet print heads
- B41J2/1604—Production of bubble jet print heads of the edge shooter type
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/16—Production of nozzles
- B41J2/1621—Manufacturing processes
- B41J2/1631—Manufacturing processes photolithography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/16—Production of nozzles
- B41J2/1621—Manufacturing processes
- B41J2/1632—Manufacturing processes machining
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/16—Production of nozzles
- B41J2/1621—Manufacturing processes
- B41J2/164—Manufacturing processes thin film formation
- B41J2/1642—Manufacturing processes thin film formation thin film formation by CVD [chemical vapor deposition]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/16—Production of nozzles
- B41J2/1621—Manufacturing processes
- B41J2/164—Manufacturing processes thin film formation
- B41J2/1646—Manufacturing processes thin film formation thin film formation by sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2202/00—Embodiments of or processes related to ink-jet or thermal heads
- B41J2202/01—Embodiments of or processes related to ink-jet heads
- B41J2202/03—Specific materials used
Definitions
- Substrate based on polycrystalline silicon for liquid jet recording head method for manufacturing the substrate, liquid jet recording head using the substrate, and liquid jet recording apparatus
- the present invention relates to a polycrystalline silicon-based substrate used for a liquid jet recording head that performs recording by discharging a recording liquid from a discharge port using thermal energy, and manufacturing of the substrate. About the method.
- the present invention further relates to a liquid jet recording head and a liquid jet recording apparatus using the substrate.
- the recording method is a non-impact recording method, and has advantages such as low noise, no particular limitation on a recording medium, and easy recording of a single image.
- a device for implementing such a liquid jet recording method that is, a liquid jet recording apparatus has a relatively simple structure, and liquid jet nozzles can be arranged at a high density, so that the speed of the recording apparatus can be increased. It has the advantage that it can be achieved relatively easily. For these reasons, the above-described liquid jet recording method has attracted public attention, and many studies have been made on the recording method. By the way, some liquid jet recording apparatuses for performing the liquid jet recording method have been marketed and put into practical use.
- FIG. 5 (A) is a cutaway perspective view of a main part of a recording head used in such a liquid jet recording apparatus
- FIG. 5 (B) is a recording head shown in FIG. 5 (A).
- FIG. 3 is a cross-sectional view of a main part along a head wave path and a plane perpendicular to a substrate.
- the recording head generally has a plurality of discharge ports 7 for discharging a recording liquid such as an ink, and corresponds to each of the discharge ports 7.
- the liquid jet recording head substrate 8 is generally provided with a heating resistor layer 2 on a substrate 1 as shown in FIG. 5 (B), and a good electrical conductivity is provided on the heating resistor layer 2.
- a wiring layer 3 made of a material having the following structure is laminated, and a portion where the wiring layer 3 is not disposed is a heating resistor 2a.
- a protective layer 4 can be provided on the liquid jet recording head substrate 8 for the purpose of covering the wirings 3a and 3b and the heating resistor 2a.
- the protective layer 4 contributes to prevention of electric corrosion and electrical breakdown of the heating resistor 2a and the wirings 3a and 3b due to contact with the recording liquid or penetration of the liquid.
- the base 1 constituting the liquid jet recording head substrate 8 a rectangular member made of a material such as single crystal silicon, glass, or ceramics can be used. However, a single-crystal silicon substrate is generally used. The reason is as follows. That is, when glass is used as the base 1, since the glass is inferior in heat conductivity, if the heating period (drive frequency) of the heating resistor 2a is increased, the heat generated by the heating resistor in the base I is increased. The ink is excessively accumulated, and as a result, the ink in the liquid jet recording head is heated by the accumulated heat, bubbles are generated, and defective ink ejection is likely to occur. When ceramic is used as the substrate 1, a substrate having a relatively large size can be manufactured, and the thermal conductivity of the substrate 1 is higher than that of glass. There is an advantage that a higher material can be selected.
- the surface of the ceramic substrate 1 is polished and smoothed to improve the adhesion of the heat-generating resistor layer 2 and to reduce the capacitance.
- alumina is generally high in hardness, there is a limit to the adjustment of the surface roughness, and this is not practical.
- single-crystal silicon wafers are optimal as a substrate for the recording head, as long as the recording head is relatively small, but the recording head is not
- the use of a single-crystal silicon wafer as the base for the increase in size causes the following inconveniences.Therefore, there is a solution for using a single-crystal silicon wafer as a base for a large recording head. It is pointed out that there is a problem to be solved.
- the single-crystal silicon substrate that is, the single-crystal silicon wafer is usually cut out from a single-crystal ingot manufactured by a single-crystal pulling method. It is formed.
- the size of a single crystal ingot that can be manufactured by this single crystal pulling method is limited to a rod shape with a diameter of 8 inches and a length of about 1 m. Therefore, there is naturally a limit to a single crystal substrate that can be obtained by cutting out from the obtained single crystal ingot. Also, if a substrate as long as possible is cut from such a single crystal ingot, the efficiency of use of the ingot becomes extremely poor, and the obtained single crystal wafer is irreversibly expensive.
- the substrate for liquid jet recording heads is better suited for recording liquids.
- a heat storage layer (lower layer) is provided directly below the heating resistor to achieve a good balance between heat storage and heat dissipation.
- the substrate is formed by thermally oxidizing the surface of a single-crystal silicon wafer cut out of the above-mentioned single-crystal ingot to form a SiO 2 heat storage layer, and forming the heat-generating resistance layer and the wiring It is manufactured by cutting individual recording heads after forming them.
- the present inventor studied to obtain a large recording head, and as shown in FIG. 9 (A), obtained a liquid jet recording head manufactured using a single crystal silicon substrate. It has been found that a problem arises in that the work-in-progress of the liquid jet recording head cut out from the end of the substrate for use deforms like a bow.
- the degree of the deformation (hereinafter referred to as “the amount of warpage” or “the degree of warpage”) reaches a maximum of 60 to 90 // m.
- the portion that causes this deformation that is, the end of the silicon wafer
- the production cost of the recording head becomes extremely high. It turned out to be.
- After a close examination of the cause of such deformation of the recording head work-in-progress it was found that such a substrate without the thermal oxidation layer as the heat storage layer had such a recording head work-in-progress. No bending deformation was found, and the above-mentioned deformation was found to be due to the thermal oxidation process.
- the deformation is caused by heat treatment of the single crystal silicon wafer, At the time of cooling, the edge of the wafer, particularly the four corners, is cooled fastest, so that tensile stress is generated at the outer edge of the substrate as shown by the arrow in FIG. B) Stress is distributed in the substrate in the state shown by the sign (+) in the figure, and a part of the wafer is cut from the wafer as shown in Fig. 9 (A) to form the substrate. Then, it was found that a part of this stress was released to cause bending deformation.
- the liquid jet recording head substrate is warped due to the stress, and the focus position is shifted during patterning. It was found that the exposure was poor and the exposure was poor. Therefore, when single crystal silicon is used as a recording head substrate, there is a natural limit in achieving a longer length. For this reason, when creating a long head to achieve higher-speed recording, it is required that a shorter recording head be connected to form an integrated liquid jet recording head unit. . However, in this case, it is very difficult to adjust the joint portion of the head so that the recorded image is not adversely affected.
- a main object of the present invention is to solve the above-mentioned problems with the conventional liquid jet recording head substrate and to use a substrate made of a specific material that enables a large recording head to be obtained. It is an object of the present invention to provide a long substrate for a head for recording a jet of a wave body. Another object of the present invention is to provide a long substrate for a liquid jet recording head using a long substrate made of polycrystalline silicon.
- Another object of the present invention is to provide a method for using the above-described single crystal silicon wafer.
- a large recording head can be achieved without integrally connecting a plurality of liquid jet recording heads as in the above case, and the liquid jet recording is performed as in the case of using a single crystal silicon wafer as described above.
- Provide the above liquid jet recording head that does not cause problems such as deformation of the head-in-process product and the accompanying deterioration in the quality of the recorded image, or exposure failure due to warpage of the liquid jet recording head substrate. Is to do.
- the present inventor has solved the above-mentioned problems in the conventional liquid jet recording head substrate and studied through the experiments described below to achieve the above object.
- the inventor has obtained the following knowledge. That is, when a polycrystalline silicon is used as a substrate of a substrate for a liquid jet recording head, (i) when the above-mentioned single crystal silicon wafer is used, a problem relating to a limitation on the size of the substrate. And a recording head capable of recording a high-quality recorded image at high speed can be provided at a low price; and (ii) a recording head can be provided on the surface of the polycrystalline silicon substrate.
- thermal oxide layer When forming a thermal oxide layer on the surface of the substrate, forming a thermal oxide layer by heat treatment, and further performing a thermal softening treatment to a thermal oxide layer softening temperature range. It has been found that the thermal oxide layer has a smooth continuous surface without any surface step, thereby providing a thermal oxide layer having good surface properties.
- the present invention has been completed based on the above findings obtained by the inventor through experiments.
- the present invention includes a liquid jet recording head substrate having the following configuration, a liquid jet recording head and a liquid jet recording apparatus using the substrate, and a method of manufacturing the substrate.
- An electrothermal transducer having a heating resistor for generating heat and a pair of wires electrically connected to the heating resistor is provided on a substrate for a wave jet recording head according to the present invention.
- a substrate for a liquid jet recording head, wherein the substrate constituting the substrate is made of polycrystalline silicon.
- the substrate for a liquid jet recording head according to the present invention can achieve extremely long substrates at a low price as compared with the case where the above-mentioned single crystal silicon wafer is used as a substrate. It has the following advantages: no deformation occurs even in a long shape, and a highly accurate wiring pattern can be easily achieved.
- a liquid jet recording head comprises: a discharge port for discharging liquid; a heat generating resistor for generating thermal energy for discharging a wave body from the discharge port; and an electrical connection to the heat generating resistor.
- the liquid jet recording head of the present invention has an advantage that a desired length can be easily achieved. That is, when the above-mentioned single crystal silicon wafer is used, the lengthening of the wave jet recording head can be achieved only by integrating a plurality of heads. No integration work is required.
- the long liquid jet recording head provided by the present invention is not suitable for recording images caused by the integration of a plurality of heads when using a single crystal silicon wafer to increase the length. There is no problem of turbulence.
- the liquid jet recording head provided by the present invention has further advantages. In other words, the yield is good because the flatness of the substrate is maintained and there is no deformation of the head-in-process product. A high-quality image can be obtained because the position of the liquid ejected from the ejection port is highly accurate.
- a liquid ejection recording apparatus includes a discharge port for discharging a liquid, a heating resistor for generating heat energy for discharging the liquid from the discharge port, and the heat energy electrically connected to the heating resistor.
- a liquid jet recording head substrate provided with an electrothermal transducer having a pair of wirings for supplying an electric signal for generating an electric signal to the heating resistor; and the electrothermal transducer of the substrate.
- a liquid jet recording head having a flow path for supplying a liquid in the vicinity of the substrate, wherein the substrate constituting the substrate is made of polycrystalline silicon; and An electric signal supply unit for supplying an electric signal to the heating resistor.
- liquid jet recording apparatus of the present invention uses the above-described liquid jet recording head, it has an advantage that high-quality recording can be performed at high speed.
- the method of manufacturing a substrate for a liquid jet recording head includes the steps of: forming a heating resistor that generates thermal energy; and an electrothermal converter having a pair of wires electrically connected to the heating resistor.
- a method for manufacturing a liquid jet recording head substrate formed on an oxide layer as a heat storage layer formed on a substrate comprising: forming a heat storage layer on the polycrystalline silicon substrate. It is characterized by forming a thermally oxidized layer having a smooth surface (hereinafter referred to as a thermally oxidized layer, a SiO 2 film, or a SiO 2 layer, as the case may be).
- the step of forming the thermal oxide layer in the method of manufacturing a liquid jet recording head substrate of the present invention is performed as described in the following (i) or ( ⁇ ⁇ ⁇ ).
- a predetermined polycrystalline silicon substrate is prepared, and the surface of the polycrystalline silicon substrate is subjected to thermal oxidation treatment to form a thermal oxide layer (that is, a SiO 2 layer). Is formed, and the formed thermal oxide layer is subjected to a thermal softening treatment to form a thermal oxide layer having a smooth surface (that is, a heat storage layer) on the polycrystalline silicon substrate.
- a predetermined polycrystalline silicon substrate is prepared, and the surface portion of the polycrystalline silicon substrate is subjected to a thermal oxidation treatment and a thermal softening treatment. The thermal oxidation layer having a smooth surface (that is, a heat storage layer) is formed on the polycrystalline silicon substrate.
- a polycrystalline silicon having a rough surface is used as a substrate, but a good thermal oxide layer is formed while ensuring the smoothness of the surface. Therefore, a desired heat storage layer equivalent to the above-described heat storage layer formed on the single crystal substrate can be formed on the polycrystalline silicon substrate. Since the heat storage layer has a good smooth surface and excellent durability, wiring and the like can be formed in a desired state on the heat storage layer. Absent.
- polycrystalline silicon members have been used in the field of solar cells.
- the polycrystalline silicon member is used as a substrate for liquid jet recording heads, so that the surface of the polycrystalline silicon member is desired because precise wiring etc. is applied on the polycrystalline silicon member. It is necessary to be in a flat condition.
- a polycrystalline silicon member has crystals of various orientations, so even if polishing is performed to obtain a mirror surface, a substrate for a liquid jet recording head is desired. It is a general recognition in the art that achieving the desired surface properties is difficult, and in the field of liquid jet recording heads, the use of polycrystalline silicon as a substrate has even been attempted. Did not.
- the inventor of the present invention ignored this recognition and dared to use polycrystalline silicon as a substrate for a liquid jet recording head substrate through an experiment described below. As a result, they have found that polycrystalline silicon can be effectively used as a substrate for a liquid jet recording head substrate.
- Mechanochemical polishing is a polishing agent for polishing, in the case of primary polishing, colloidal silica to which various alkalis such as NaOH, oxygen, organic amine, etc. are added, and secondary polishing.
- colloidal silica For polishing, use is made of colloidal silica with ammonia added.
- a single crystal substrate sample was prepared as follows. First S i HC 1 residual impurity concentration created by hydrogen reduction and precipitation reaction by thermal decomposition of 3 was dissolved those Yabu ⁇ high purity polycrystalline port head below 1 PP b, in the CZ method ⁇ 1 1 1> From a boron-doped P-type single crystal ingot (8 inch x 110 cm) manufactured by pulling up in the direction, it is shaped into a prism by a grinder, and then shaped into a plate using a multi-wire saw. Cut out. Next, the surface layer was removed and flattened by about 30 / m by lapping.
- the sample of the polycrystalline silicon substrate is a high-purity polycrystalline silicon II produced by hydrogen reduction and thermal decomposition used for the production of a single-crystal silicon, and a single-crystal silicon crushed sample.
- a quartz crucible After being heated and melted at 1420 ° C with a quartz crucible, it was poured into a graphite mold and cooled to form a 40 cm square ingot. Next, the ingot was cut into a plate shape using a multi-wire saw. Next, the surface was removed by lapping and the surface was flattened to about 30 / m.
- 300 (mm) x 150 (mm) x 1.1 (mm) (hereafter abbreviated as 300 x 150 x 1.1 (mm) for simplicity) Samples were placed on each of single-crystal silicon and polycrystal silicon. As shown in Table 1, several were prepared.
- a single-side polishing machine manufactured by Speed Fam Co., Ltd. was used as a polishing machine.
- the polishing process was divided into primary polishing and secondary polishing under the following conditions, and the presence / absence of addition of aluminum alloy during the primary polishing and the surface finishing performance were evaluated. Table 1 summarizes the evaluation results.
- Polishing cloth Polishing cloth; Polyurethane impregnated polyester nonwoven fabric, Abrasive; Colloidal force (particle diameter 0.06 ⁇ ), Polishing pressure: 250 g / cm 2 , Polishing temperature: 42 ° C, Processing speed 0.ma fi m / min
- polishing cloth suede-type foamed polyurethane, abrasive; silica fine powder (0.01 ⁇ ), polishing pressure: 1775 g Zcm 2 , polishing temperature: 32 ° C, processing speed: 0.2 ⁇ m / min
- a substrate sample of single crystal silicon was prepared as follows. That first melted those Yabu ⁇ the S i HC 1 3 high-purity polycrystalline silicon hob head residual impurity concentration created by hydrogen reduction and precipitation reaction by thermal decomposition of less than 1 PP b of at CZ method ⁇ 1 From a P-type single crystal ingot (8 inch x 110 cm) obtained by pulling up in the 1 1> direction, it was shaped into a prism using a grinder, and then turned into a square shape using a multi-wire saw. I cut it out.
- the edge is chamfered with a beveling machine and then polished.
- a final surface finish was carried out by a polishing process to obtain a mirror-finished substrate having a surface roughness R max of 150 A.
- the surface of the substrate was thermally oxidized by a pyrogenic oxidation method (hydrogen combustion oxidation method) as schematically shown in FIG.
- the oxidation is performed, for example, as follows. That is, hydrogen and oxygen are introduced into the substrate quartz tube 7 3 you thermally oxidized separately produced H 2 0 reacts with the quartz tube 7 within 3, residue is burned.
- a base 71 for performing a thermal oxidation treatment is arranged in the quartz tube 73 and heated by an electric furnace 74.
- the thermal oxidation of the prepared substrate is performed by the above-described oxidizing apparatus and method, by introducing oxygen under the following conditions: gas pressure: 1 atm, processing temperature: 1150, processing time: 14 hours. A 3 m thermal oxide layer was obtained.
- a polycrystalline silicon substrate sample is a high-purity polycrystal produced by the precipitation reaction by hydrogen reduction and thermal decomposition used for the production of a single crystal, or a crushed single crystal.
- a single crystal or a crushed single crystal.
- a plate-like polycrystalline silicon was cut out of this ingot at a position such that the average crystal grain size was 2 mm by a multi-wire machine.
- the surface layer is removed and flattened, the edge is chamfered with a beveling machine, and the final surface is polished to finish the surface. Finished to a mirror substrate of 150 A.
- thermal oxidation was carried out by the above-mentioned pyriogenic method under the same conditions as above to form a 3 m-thick thermal oxide layer.
- six polycrystalline substrate samples having the dimensions shown in Table 2 were prepared.
- an aluminum layer (450 A) as a wiring, a hafnium boron as a heating resistor; f B 2 layer (150 A), T i layer (50 A) as an adhesion improving layer with the upper protective layer, S i 0 2 (1.5 ⁇ .), T a (500 OA) and polyimide (3 ⁇ each) were laminated to form six substrates.
- the next step is to laminate a 20-jm-thick negative dry film to form the flow path and pattern the flow path by exposing it.
- the degree of warpage was evaluated for each of the obtained substrates. The degree of warpage was determined by placing the sample on a surface plate and measuring the maximum displacement using a dial gauge with a minimum scale of 1 zm. Table 2 shows the results.
- Table 2 show that the maximum warpage of a polycrystalline silicon substrate sample with a sample size of 300 x 150 x 1.1 (mm) was 1, and the other samples had the maximum warpage. It is a relative value of the quantity.
- the polycrystalline silicon substrate sample showed only the same amount of warpage at all sizes used in the experiment, whereas the single crystal silicon substrate sample did not.
- the increase in the amount of warping was observed from the sample size of 500 ⁇ 150 ⁇ 1.1 (mm), and the relative value of the amount of warpage was 3 for the sample size of 800 ⁇ 150 ⁇ 1.1 (mm);
- the relative amount of 2 when the actual exposure is performed, considerable exposure failure occurs due to the shift of the focus position, and with the relative amount of warpage of 3, all of the exposure becomes poor; and the single crystal silicon substrate sample.
- a sample size of 500 x 150 x 1.1 (mm) is the limit at which a liquid jet recording head can be manufactured.
- the selection of the crystal grain size for the substrate is based on the fact that, in the case of a polycrystalline silicon ingot, the crystal grain size increases from the surface in contact with the ⁇ shape toward the center, so that the ingot is cut out from this ingot.
- a plurality of substrates (sample Nos. 2 to 8) having the average crystal grain size shown in the section of Sample No. 2 to 8 in Table 3 were obtained. I got it.
- the average crystal grain size of the substrate was measured by a crystal grain size measurement method according to the cutting method described in the section of Ferrite grain size test method for steel of JIS G552.
- the surface of each of the prepared single-crystal silicon substrate (sample No. 1) and polycrystalline silicon substrate was 3 ⁇ m thick by pyrodynamic oxidation method as described in Experiment B. A thermal oxide layer was formed.
- the prepared sample was placed on a precision XY table with a linear scale, and the maximum warpage was measured.
- Figures 9 (B), 9 (C) and 9 (D) show explanatory diagrams of the method of measuring the amount of warpage employed in this case.
- the polycrystalline silicon substrate has less deformation due to warpage than the single crystal silicon substrate.
- those having an average crystal grain size exceeding 8 mm have little advantage over single crystal silicon, and have an average crystal grain size exceeding 2 mni and an average crystal grain size of 8 mni or less. It was found that, though having an advantage over single-crystal silicon, those with an average crystal grain size of 2 mm or less were inferior. From this, it was found that the average crystal grain size of the polycrystalline silicon base was preferably 8 mm or less, and more preferably 2 mm or less.
- the substrate constituting the liquid jet recording head substrate is required to have a smooth surface in a desired state because wiring is provided on the substrate. Therefore, it is necessary to satisfy this requirement even when the substrate is made of polycrystalline silicon.
- polycrystalline silicon is used in the field of solar cells.
- the substrate constituting the substrate for the wave jet recording head is described. Table as in the case of There are no severe requirements for surface smoothness.
- polycrystalline silicon substrates used for solar cells usually contain inclusions. That is, the polycrystalline silicon ingot used for obtaining the polycrystalline silicon substrate for a solar cell melts the silicon in a quartz crucible and cools and solidifies the molten silicon. It is manufactured by doing so. The silicon melt is chemically very active, and also reacts with quartz, which is a constituent material of the crucible material, as SiO 2 + Si ⁇ 2Si 0.
- the silicon firmly adheres to the inner wall of the crucible during cooling and solidification. Cracks tend to be formed in the crucible when strain is applied to the material due to the difference in thermal expansion coefficient between quartz and silicon. Therefore, when an ingot is taken out of the crucible, a powdery release agent is applied to the inner wall surface of the crucible so that the ingot can be easily taken out. For this reason, the release agent inevitably intervenes in the polycrystalline silicon ingot. Such inclusions are not a problem in solar cells. However, when wiring is provided on a substrate made of such a polycrystalline silicon, first, the surface of the substrate is polished and mirror-finished, and the inclusions become defects such as pit / projections of several tens / zm.
- the base constituting the liquid jet recording head substrate is contained in the polycrystalline silicon when it is composed of polycrystalline silicon.
- the effects of inclusions were examined from a quantitative point of view.
- a single crystal of dimensions 330 ⁇ 150 ⁇ 1.1 (mm) was formed from the single crystal silicon wafer formed.
- the substrate was cut out, subjected to lapping and polishing, and finished to a mirror-finished substrate having a surface roughness of R max 150A .
- This substrate was used as Sample 1.
- the surface condition of the substrate (Sample 1) was observed with a substrate surface inspection device using CCD reading method (trade name: Scantech, manufactured by Nagase & Co., Ltd.).
- the number of defects per area of the substrate was 1 Zcm 2 or less at all measurement points in the range of 1 m or more in diameter, since there was no inclusion of the release agent.
- the results are shown in Table 4.
- a 50 cm square polycrystalline silicon ingot was made after melting the silicon in a quartz crucible without the release agent applied to the inner surface. From this ingot, a polycrystalline silicon substrate of the same dimensions as a single-crystal silicon substrate is cut out, and its surface is wrapped and polished to a mirror surface substrate with a maximum surface roughness of 150 A. Was. This substrate was used as Sample 2. The surface condition of the substrate was observed in the same manner as in the case of the single crystal silicon substrate (sample 1). As a result, since there was no inclusion of the release agent, the number of defects per area of the substrate was 1 piece / cm 2 or less at all measurement points in the range of 1 ⁇ ⁇ or more in diameter of detection capability. The results are shown in Table 4.
- a plurality of substrates were prepared by performing the same operation as in the case of preparing sample 2 except that a release agent was used.
- the amount of the release agent used was different for each sample.
- the surface condition of each of the obtained substrates (samples 3 to 6) was observed in the same manner as in the above single crystal silicon substrate (sample 1).
- the number of defects in each of the samples 3 to 6 was 5 cm 2 or less, 10 ( ⁇ 11 12 or less, 50 Z cm 2 or less, 100 (: 111 2 or less)
- the surface of each of the substrates was subjected to a thermal oxidation treatment in the same manner as in the experiment B, to obtain a thermal oxide layer of about 3: 1.
- test wiring to detect disconnection or short circuit due to inclusions As a pattern, an Al film was formed on the thermal oxide layer of each sample to a thickness of 450 by magnet sputtering, and the wiring width was 20 ⁇ m. Im folded wiring pattern was created. At this time, the number of folded wirings for each sample was assumed to be the wiring pattern of the liquid jet recording head, and the test pattern was 8 mm in wiring length and 4 736 in the number of wirings. This test pattern was created for each sample.
- the continuity test was performed by bringing the probe pins into contact with the ends of each wiring.
- the conduction test was evaluated on the basis of a test in which no disconnection or short circuit was found.
- the number of patterns having no disconnection or short circuit for 15 test patterns that is, the number of acceptable patterns Z15 test patterns was expressed as a yield. The results obtained are shown in Table 4.
- a polycrystalline silicon member that can be used effectively as a substrate constituting a liquid jet recording head substrate has a smoothness (smooth state) on its surface, and preferably has a diameter equal to or larger than the diameter.
- the number of defects should be 10 or less Z cm 2 , and more preferably, the number of defects having a diameter of lum or more should be 5 or less Z cm 2 .
- the present inventor uses a polycrystalline silicon substrate in place of the single crystal silicon substrate, and thermally oxidizes the surface portion of the polycrystalline silicon substrate to form a heat storage layer in the same manner as in the case of forming the heat storage layer.
- i 0 2 layers were formed, were observed surface condition of the S i 0 2 layers. As a result, it was found that a step of about several thousand A at maximum occurred between crystal grains on the surface of the SiO 2 layer.
- the two layers do not function as the desired heat storage layer, and are not practical from an economic viewpoint.
- the inventor tried to form the heat storage layer (that is, the SiO 2 layer) by a vacuum film forming method, that is, each of a sputtering method, a thermal CVD method, a plasma CVD method, and an ion beam evaporation method.
- a vacuum film forming method that is, each of a sputtering method, a thermal CVD method, a plasma CVD method, and an ion beam evaporation method.
- the film thickness becomes uneven, it takes a long time to form a film, and dust generated during the film formation enters the film and causes damage due to cavitation.
- Protrusions with a diameter of a few microns were formed. It was also found that the occurrence of these protrusions caused current to leak from them, causing electrical short circuits. For this reason, the vacuum deposition method uses the heat storage layer (that is,
- the present inventors have tried to form the thermal storage layer (S i 0 2 layers) employ respective spin-on-glass method and the de-up pulling method, even in cases, made form Since the film quality of the SiO 2 layer is poor, it is difficult to achieve good film quality, and impurity particles may be mixed in the film, and none of these film forming methods can be adopted. I found it.
- a flattening process is employed as a technique for improving the problem of disconnection at a step portion of a multilayer wiring.
- a planarization process widely used in MOS LSIs is a reflow technology for PSG films.
- This technique lowers the softening point of the PSG film as the interlayer insulating film between Serco contain S i 0 2 film P 2 0 5 of several mol% in which are formed, for example, CVD method, heat treatment (reflow treatment) By doing so, the steps of the PSG film are flattened.
- the reflow temperature at this time is about 800 to 100 ° C. in consideration of the influence of heat on the formed wiring and the like.
- the substrate constituting the liquid jet recording head substrate is made of polycrystalline silicon, and the thermal oxidation layer formed on the polycrystalline silicon substrate is In order to eliminate the above-mentioned step, the above-mentioned flattening process cannot be adopted.
- the recording head is provided with the recording head.
- the heating resistor When performing recording by using, the heating resistor generates heat at about 110 o ° c to generate thermal energy for discharging the recording liquid, so it has characteristics that can withstand this temperature sufficiently. Is required. Therefore, it is essential that the base constituting the substrate satisfies this requirement.
- the substrate is formed of a polycrystalline silicon completely different from the PSG film in the semiconductor device, and a thermal oxide layer is formed on the polycrystalline silicon substrate, as described above, A step occurs on the surface of the oxide layer.
- the present inventor has tried the above-described step-elimination method in the semiconductor device to eliminate the step, but could not achieve the object. This point is clear from the experimental results described below. That is, even if a reflow processing temperature (about 110 ° C.) which is much higher than the upper limit (about 100 ° C.) of the reflow processing temperature used when eliminating the step in the semiconductor device described above is used. The surface step of the thermal oxidation layer could not be eliminated.
- the substrate forming the liquid jet recording head substrate is made of polycrystalline silicon, and the step on the surface of the thermal oxide layer formed on the polycrystalline silicon substrate (ie, There is no effective way to eliminate surface steps).
- the present inventor tried through an experiment described below to solve the problem of the occurrence of steps on the surface of the thermal oxide layer through a thermal softening treatment. That is, in the following experiments, the present inventor outlines two techniques: (i) performing a thermal oxidation treatment on the surface portion of the polycrystalline silicon substrate to form a thermal oxide layer; Attempts were made to apply a thermal oxidation treatment to the layer, and (ii) to simultaneously apply a thermal oxidation treatment and a thermal oxidation treatment to the surface of the polycrystalline silicon substrate.
- the following describes (a) the reason why the thermal oxidation layer (SiO 2 layer) formed when the surface of the polycrystalline silicon substrate is subjected to thermal oxidation treatment has a surface step, and (b) ) The surface of the polycrystalline silicon substrate having the step subjected to the thermal oxidation treatment is subjected to thermal softening treatment in the softening temperature range of the thermal oxide layer, so that the SiO 2 layer having no surface step is formed.
- the reason why the present inventors have formed through experiments on the surface of the polycrystalline silicon substrate will be described with reference to FIGS. 4 (A) to 4 (C).
- the thermal oxidation process of the surface of the polycrystalline silicon substrate is examined.
- a linear rule is established between the thickness of the thermal oxide layer 1'3 and the oxidation rate.
- the reaction of oxygen (0 2) at the interface between the polycrystalline silicon oxide silicon constituting the (S i) and the thermal oxide layer (S i 0 2) is rate-limiting.
- the oxidation rate of oxygen varies depending on the orientation of the crystal plane.
- the rate at which oxygen diffuses through the thermal oxide layer 13 is limited. It is considered that the diffusion rate of oxygen in the thermal oxide layer 13 does not depend on the orientation of the crystal plane of the silicon crystal grains 12.
- the step on the surface of the thermal oxide layer (that is, the thermal oxide film) 13 for each crystal grain 12 of the polycrystalline silicon substrate 11 occurs at the very beginning of the thermal oxidation process, and to some extent It can be considered that the step does not increase after the formation of the thermal oxide layer 13 proceeds.
- the surface state of the thermal oxide layer is deformed by applying heat so that the surface steps of the thermal oxide layer are averaged to become a smooth surface. Concentration of the cavitating mesh on the body is eliminated and durability is improved.
- the present invention unlike the case of flattening the interlayer insulating film on the wiring at the time of forming the multilayer wiring in the LSI manufacturing process, it is the flattening of the surface step of the thermal oxide layer formed on the polycrystalline silicon. It is possible to achieve smoothing with less fluidity.
- the above-mentioned thermal softening treatment may be performed after the thermal oxidation treatment (that is, formation of the thermal oxide film), or may be performed simultaneously with the thermal oxidation treatment.
- the thermal aging treatment it is also possible to introduce a predetermined impurity into the polycrystalline silicon substrate to be used and perform the thermal aging treatment.
- impurities the curing temperature of the thermal oxide layer is lowered, and the processing efficiency can be improved. In other words, the temperature for aging can be relatively low, and the processing time can be reduced.
- the softening treatment is performed at a relatively high temperature, the softening of the thermally oxidized layer proceeds effectively, so that the steps can be more effectively smoothed.
- the thermal oxide layer formed on the polycrystalline silicon substrate by advancing the softening state of the thermal oxide layer The adhesion to the formed heating resistor is improved.
- the present inventors studied the effect of a polycrystalline silicon substrate having a thermally oxidized layer formed by performing the above-described thermal softening treatment subsequent to the thermal oxidation treatment by preparing a liquid jet recording head substrate. did.
- a polycrystalline silicon ingot having an average crystal grain size of about 2 mm was prepared by the casting method described above. Five plate-like substrates were cut out from the obtained ingot. Each substrate was lapped and polished to obtain a mirror substrate with a size of 300 x 150 x 1.1 (mm) and a surface roughness of R max 15 OA. The substrate was used. Next, the thermal oxidation treatment was performed on the surface of the polycrystalline silicon substrate by the same method and conditions as in Experiment B except that the tube (see 73 in FIG. 7) was made of SiC. Was formed.
- Each of the five polycrystalline silicon substrates having the thermal oxide layer thus obtained was introduced into a thermal oxidation furnace, and the furnace temperatures were set to 1380 ° C, 1330 ° C, and 1280, respectively. C, 1 2 3 0. C, the temperature was kept at 118 ° C. for 1 hour to perform a thermal softening treatment on the thermal oxide layer.
- polycrystalline silicon substrates of samples N 0.1, 2, 3, 4, and 5 were prepared.
- a polycrystalline silicon substrate having a heat storage layer formed of a thermal oxide film (SiO 2 film) on the surface was obtained.
- the thickness of the formed heat storage layer (that is, the SiO 2 layer) was 3.0 zm in each case.
- Measuring position A total of 15 intersection points of a line segment dividing the short side 150 mm of the substrate into four equal parts and a line dividing the long side 300 mm into six equal parts.
- Evaluation criteria 15 The maximum height of the step in the 5 locations was 0 m or more and less than 0.05 ⁇ , ⁇ was 0.05 m or more and less than 0.1 m, and X was 0.1 / m or more. .
- the surface of the heat storage layer using the Photo Li lithography technology, consisting of H f B 2 heating A resistor [Size: 20 / mx 100 0 ⁇ ⁇ Thickness: 0.16 / Am. Wiring density: 16 Pel (ie 16 wires / mm)] and A connected to each heating resistor An electrode consisting of 1 (width 20 m, thickness 0.6 / ⁇ ) was formed. Further, the coercive Mamoruso consisting S i 0 2 ZT a formed by Supattari ring on the heat generating resistor and electrode were formed portion are shown in 1 (A) Figure and the 1 (B) Fig. A liquid jet recording head substrate with the above configuration was created.
- sample No. 1 The substrate of sample No. 1 was deformed due to the excessively high thermal aging temperature, and the substrate cracked when applying a photoresist over the roll coat in the liquid jet recording head manufacturing process. As a result, it was not possible to produce a liquid jet recording head.
- thermo oxidation layer thermal storage layer
- Five mirror-finished substrates having a size of 300 ⁇ 150 ⁇ 1.1 (mm) and a surface roughness of R max 15 OA were prepared in the same manner as in Experiment E-1. These were used as polycrystalline silicon substrates (samples N 0.6 to 10).
- a thermal storage layer thermal oxidation layer was simultaneously applied to each of these polycrystalline silicon substrates using the same apparatus as used in Experiment E-1. Formed.
- each polycrystalline silicon substrate is placed in a thermal oxidation furnace, oxygen is introduced therein by a pyrogenic method, and the inside of the thermal oxidation furnace is maintained at a predetermined temperature to thereby prepare the polycrystalline silicon substrate.
- a thermal storage layer thermal oxide layer, ie, SiO 2 layer
- the furnace temperature at that time was set to 1380 ° C, 1330 ° C, 1280 ° C, 1230 ° C, and 1180 ° C, which were different in each case.
- Thermal storage layer thermal acid The heating times were 5, 7, 8, 11, and 14 hours, respectively, in order to obtain 3 m of the modified Si0 2 layer).
- five polycrystalline silicon substrates of samples N0.6 to N10 were prepared.
- a polycrystalline silicon substrate having a heat storage layer made of a thermal oxide film (SiO 2 film) formed on the surface was obtained.
- the thickness of the formed heat storage layer (that is, the SiO 2 layer) was 3.0 im in each case.
- the substrate of sample No. 6 was deformed due to the excessively high thermal aging temperature, and the substrate cracked when applying a photoresist over the roll coat in the liquid jet recording head manufacturing process. As a result, it was not possible to produce a liquid jet recording head.
- a wave path and a liquid chamber were formed by a dry film or the like on the formed heat storage layer, and a discharge port was formed by cutting a slicer.
- One liquid jet recording head having the configuration shown in Fig. 5 and Fig. 5 (B) was created.
- a driving pulse (print signal) having a pulse width of 1.1 Vth (Vth is a foaming voltage) and a pulse width of 10 s was repeatedly applied to the heating resistor for each of the four obtained liquid jet recording heads. Ink was discharged from each discharge port to perform a discharge durability test.
- the thermal oxidation treatment was performed on the surface of the polycrystalline silicon substrate to form a thermal oxidation layer (heat storage layer), and the thermal oxidation treatment was performed on the thermal oxidation layer. Then, the effect of doping the thermal oxide layer formed by the thermal oxidation treatment with an impurity and performing the thermal softening treatment on the impurity-doped thermal oxide layer was examined. ⁇
- the doping of impurities to the surface of the thermal oxide layer was performed by the normal pressure CVD method.
- the dopant using a POC 1 3 liquid source, it is introduced into the furnace in a carrier N 2 gas was kept in a saturated state.
- the diffusion time was set to 30 minutes, and the diffusion temperature was set to 1550 for samples No. 11 to 15. C, 100 ° C. for samples No. 16 to 20 and 9500 for samples No. 21 to 25.
- the phosphorus concentration on the surface was measured using a secondary ion mass spectrometer (model name: IMS-3F, manufactured by CAMECA) (hereinafter abbreviated as SIMS).
- a polycrystalline silicon substrate having a heat storage layer formed of a thermal oxide film (SiO 2 film) on the surface was obtained.
- the thickness of the formed heat storage layer (that is, the SiO 2 layer) was 3.0 m in each case.
- the heating resistor consisting of H f B 2 [Size: 2 0 ⁇ mxl 0 0 ⁇ m, thickness: 0.16 im, wiring density: 16 Pel (that is, 16 lines Zmm)] and an electrode consisting of A 1 connected to each heating resistor (width 2 0 zm, thickness 0.6 m).
- a protective layer made of S i 0 2 / T a formed by spatter-rings on the heat generating resistor and electrodes are formed portion, first 1 (A) Figure and the 1 (B) Fig.
- a substrate for a liquid jet recording head having the structure shown in Fig. 1 was prepared.
- a wave path and a liquid chamber are formed on the substrate by a dry film or the like, and a discharge port is formed by cutting a slicer.
- a discharge port is formed by cutting a slicer.
- Thermal oxidation layer (S i 0 2 layers), at ⁇ temperature 1 1 3 0, or even on more than, if you doped with an impurity so that the temperature as low as possible, as compared with the case of not doping Steps can be effectively eliminated at a temperature lower than 100 ° C and the operating temperature of the processing furnace can be made relatively low, so that the life of the furnace is prolonged and the production cost is advantageous.
- the upper limit of the aging temperature is lower than 133 ° C., as in Experiments E-1 and E-2, where no adverse effect is caused by the deformation of the polycrystalline silicon substrate.
- the oxidized state of the thermally oxidized layer is further advanced, and the surface state of the thermally oxidized layer is more preferably a step having been eliminated.
- a special feature of the present invention resides in the base constituting the substrate for the recording head for corrugated recording.
- the substrate is made of polycrystalline silicon, and is distinguished by having a heat storage layer (thermal oxide layer) having a smooth surface property on the surface of the polycrystalline silicon.
- the heat storage layer is a surface portion of the polycrystalline silicon. It is formed by applying a thermal oxidation treatment and a thermal softening treatment to each of them.
- the surface of the substrate is generally not flat because of its crystal grains, and as described in the above-described experiment, the thermal oxidation layer formed on the surface is generally used. Has a surface with steps.
- a polycrystalline silicon substrate having a heat storage layer having a smooth surface property is prepared by preparing a substrate made of polycrystalline silicon and subjecting a surface portion of the substrate to thermal oxidation treatment and thermal treatment. This is realized by forming a heat storage layer having a smooth surface with no steps on the surface of the substrate by performing the softening treatment.
- the polycrystalline silicon substrate having such a heat storage layer is used as a component of a substrate for a liquid jet recording head, the substrate is heated or cooled by using the substrate. Even if internal stress is generated due to non-uniform shrinkage, deformation does not occur as much as is actually a problem.
- the thermal softening treatment may be performed after a thermal oxidation treatment is performed on the polycrystalline silicon substrate to form a thermal oxidation layer (heat storage layer), or may be performed simultaneously with the thermal oxidation treatment. May be. When the thermal oxidation treatment and the thermal softening treatment are performed simultaneously and in parallel, these treatments are performed separately to form a desired heat storage layer on the polycrystalline silicon substrate, which is much longer than the time required for forming the desired heat storage layer. Shorter.
- thermal softening treatment independently, for example, Harogenra lamp, lamp heating or C 0 2 such as a xenon lamp, YAG, continuous wave heating or pulse oscillation heating by Les one
- Harogenra lamp, lamp heating or C 0 2 such as a xenon lamp, YAG, continuous wave heating or pulse oscillation heating by Les one
- the heat softening treatment may be performed only on a desired portion of the surface of the polycrystalline silicon substrate, for example, only on the portion where the heating resistor is formed, by continuous oscillation heating, pulse oscillation heating, high frequency heating, or the like using a beam. .
- the heat softening treatment is performed at a temperature lower than the melting temperature of the base material, polycrystalline silicon. It is necessary to perform at a low temperature. Specifically, the temperature at this time is desirably selected in the range of 1230 ° C to 1330 ° C, as clarified in Experiment E.
- the thermal oxidation treatment and the thermal softening treatment are performed separately, impurities are introduced into a thermal oxide layer formed by performing the thermal oxidation treatment, and then the thermal oxidation is performed on the thermal oxide layer doped with the impurities.
- the heat treatment can be performed at a temperature lower than the temperature in the heat treatment when no impurities are used.
- impurities introduced into the thermal oxide layer impurities generally used in the technical field of semiconductors, such as P, B, and As, can be selectively used.
- an impurity introduction method employed in semiconductor technology can be employed.
- the concentration of impurities introduced into the thermal oxide layer varies depending on the type of impurities used. In general, the upper limit of the concentration is determined so that the heat storage layer is not softened by the temperature at which the heating resistor formed on the heat storage layer (thermal oxidation layer) generates heat. It is appropriately determined by taking into consideration that the surface is oxidized to a desired state by the aging treatment to provide a smooth surface.
- the thermal aging treatment performed in the present invention is mainly performed for the purpose of eliminating the steps on the surface of the thermal oxide layer and obtaining a smooth surface state.
- the heat-generating resistor formed on the desired smooth surface of the desired thermal oxide layer formed by performing the thermal softening treatment ensures the desired adhesion to the thermal oxide layer.
- the present invention provides a liquid jet recording head substrate using the above-described substrate based on polycrystalline silicon, a liquid jet recording head equipped with the recording head substrate, and the recording head. And a method for manufacturing the liquid jet recording head substrate.
- the configuration of each of these is as outlined and described below.
- a liquid jet recording head substrate provided by the present invention is provided on a substrate based on the above-mentioned polycrystalline silicon, a heating resistor for generating heat and an electrical connection to the heating resistor. Having a pair of wires A substrate provided with a gas-to-heat converter, characterized in that the surface of the substrate has an oxide layer formed by performing a thermal oxidation treatment and a thermal softening treatment.
- a liquid jet recording head provided by the present invention includes: a discharge port for discharging a liquid; a heat generating resistor for generating heat energy for discharging the liquid from the discharge port; A liquid jet recording head substrate, which is electrically connected to the body, and includes an electrothermal transducer having a pair of wirings for supplying an electric signal for generating the thermal energy to the heating resistor; A liquid jet recording head having a flow path for supplying a recording liquid near the electrothermal transducer of the substrate, wherein the substrate is a base based on polycrystalline silicon. And an oxide layer formed by performing a thermal oxidation treatment and a thermal softening treatment on the surface of the substrate.
- the liquid jet recording apparatus includes: (a) a discharge port for discharging liquid, a heat generating resistor for generating heat energy for discharging liquid from the discharge port, A liquid jet recording head, which is electrically connected to a resistor and includes an electrothermal converter having a pair of wirings for supplying an electric signal for generating the thermal energy to the heating resistor.
- a substrate and (b) a flow path for supplying a recording liquid in the vicinity of the electrothermal converter of the substrate, wherein the substrate (a) comprises a substrate based on polycrystalline silicon. Wherein the substrate has an oxide layer formed on the surface thereof by a thermal oxidation treatment and a thermal softening treatment.
- a method of manufacturing a substrate for a liquid jet recording head is directed to an electric heating device having a heating resistor for generating thermal energy and a pair of wirings electrically connected to the heating resistor.
- a method for manufacturing a substrate for liquid jet recording head wherein a conversion body is formed on a substrate, wherein a substrate composed of polycrystalline silicon is used as a substrate constituting the substrate.
- a substrate typically used as a substrate constituting a liquid jet recording head substrate and typically composed of polycrystalline silicon (hereinafter simply referred to as a “polycrystalline silicon substrate”) is As described in the above experiment, it is easy to increase the length of the recording head, which is difficult to achieve when using a single-crystal silicon substrate, because deformation is less likely to occur than a single-crystal silicon substrate. It has a remarkable effect of being able to do so.
- the substrate can be easily made to have a desired length, and in that case, As described in Experiment B above, since the degree of warpage is smaller than that of a single-crystal silicon substrate, a long recording head hardly affected by warpage can be easily achieved. In addition, in the long recording head, there is no occurrence of pixel disturbance that occurs when a plurality of small recording heads are integrally connected to form a long recording head.
- the amount of warpage is proportional to the average crystal grain size of the polycrystalline silicon substrate, as clarified in Experiment C described above. Due to the demand for improved yield in the production of recording heads, the preferred average crystal grain size of polycrystalline silicon as a base constituting the substrate for liquid jet recording heads is 8 mm or less, and more preferable average crystal grains. The diameter is less than 2 mm. When a polycrystalline silicon substrate having an average crystal grain size in such a range is used, there is no problem of warpage of the substrate, and a long liquid jet that can obtain a high-quality recorded image at a high speed. A recording head substrate can be easily achieved.
- the number of defects having a diameter of 1 ⁇ m or more is preferably 10 or less Z cm 2, and more preferably 5 or less cm 2 .
- FIG. 1 (A) is a schematic plan view of a main part of an example of a liquid jet recording head substrate of the present invention.
- FIG. 1 (B) is a cross-sectional view taken along line X--X 'of FIG. 1 (A).
- FIG. 2 is a schematic cross-sectional view of a base constituting the liquid jet recording head substrate.
- a liquid jet recording head substrate 8 is formed on a polycrystalline silicon substrate 1 by a heating resistor that generates thermal energy for jetting a recording liquid.
- the heating resistor 2a and the wirings 3a and 3b are formed on the substrate 1 by, for example, sputtering, a heating resistor layer 2 made of a material having a certain volume resistivity, and an electric conductive layer. It is formed by laminating an electrode layer 3 made of a good material and then patterning it into a predetermined shape by a photolithographic process.
- the heating resistor by applying an electric signal to the heating resistor via the wirings 3a and 3b, the heating resistor generates heat.
- Desirable materials for forming the heating resistor layer hafnium boride (H f B 2), tantalum nitride (T a 2 N), oxide Rubijiyuumu (R u 0 2), T a - A 1 alloy, T a —
- Various metals, alloys, metal compounds, cermets, etc. including A1-Ir alloys are used.
- wiring layer 3 is As a material to be formed, a highly conductive metal such as aluminum or gold can be used.
- the liquid jet recording head substrate 8 is provided with a protective layer 4 so as to cover the wirings 3a and 3b and the heating resistor 2a.
- the protective layer 4 is provided for the purpose of preventing the heat generating resistor 2a and the wirings 3a and 3b from being electrically corroded and electrically destructed due to the permeation of the contact ink with the ink.
- Protective layers were do this, S i 0 2, S i C, can be ⁇ an electrically insulating material such as S i 3 N 4.
- the protective layer may have a multilayer structure. In that case, for example, it may be with the conductive protective layer by laminating a layer composed of T a and T a 2 0 5 on the configured layer with stunned ⁇ fee.
- the direction in which the liquid is ejected from the ejection port is substantially the same as the direction in which the liquid is supplied to the heating resistor.
- the two directions are different from each other (for example, substantially perpendicular).
- the liquid jet recording head of the present invention also includes the present invention.
- an embodiment of a liquid jet recording head using the above-described substrate will be described.
- a liquid path 6 for supplying an ink serving as a recording liquid is formed near each of the heating resistors 2a by connecting the top plate 5 to a substrate. Then, the ink in the liquid path is heated by the respective heating resistors to generate bubbles, and the ink is ejected from the ejection port 7 by the pressure of the bubble generation to perform printing.
- FIGS. 5 (A) and 5 (B) show a liquid jet recording head having a one-to-one correspondence between the number of heating resistors and the number of ejection ports.
- the recording head of the present invention is not limited to this. That is, any form in which the above-described substrate can be applied, such as a form in which a plurality of heating resistors correspond to one discharge port, is an embodiment of the present invention. Also, in FIGS. 5 (A) and 5 (B), the configuration is such that the substrate surface on which the heating resistor is disposed is substantially parallel to the direction in which the ink is discharged. However, the present invention is not limited to this, and it goes without saying that the direction in which ink is ejected and the substrate surface may intersect.
- the liquid jet recording head of the present invention is a recording head which is incorporated in the apparatus or is detachable from the recording apparatus, and is supplied with ink from the ink via a tube or the like.
- the recording head may be a recording head that is detachable from the recording device and that is detachably connected to the ink tank.
- Various recording liquids can be used as the recording liquid applicable to the recording head of the present invention, but generally, 0.5 to 20 wt% of a dye, a (polyhydric) alcohol, a polyalkylene glycol, and the like.
- a water-soluble organic solvent such as coal having an ink composition of 10 to 80 wt% and water of 10 to 90 wt% can be preferably used, and as an example of a specific ink composition, Can be cited as a composition of C.I. hood black 23 wt%, diethylene glycol 25 wt%, N-methyl-2-pyrrolidone 20 wt%, and water 52 wt%. .
- FIG. 6 is an external perspective view showing an example of an ink jet recording device (IJRA) in which the recording head according to the present invention is mounted as an ink head cartridge (IJC).
- IJRA ink jet recording device
- IJC ink head cartridge
- reference numeral 120 denotes an ink jet head cartridge (IJC) having a nozzle group for discharging ink while facing the recording surface of the recording paper fed onto the platen 124.
- Reference numeral 116 denotes a carriage HC that holds the IJC 120.
- the carriage HC is connected to a part of the drive belt 118 that transmits the driving force of the drive motor 117, and is arranged in parallel with each other. By making it slidable with the guide shafts 119A and 119B, it is possible to reciprocate over the entire width of the IJC120 recording paper.
- an ink cartridge with a small recording head is used as the recording head.
- the long recording head of the present invention such as a full line type capable of recording according to the width can be used, and such a long recording head can be used.
- a recording device can be obtained.
- Reference numeral 126 denotes a head recovery device, which is provided at one end of the movement path of the IJC 120, for example, at a position facing the home position. The head recovery device 126 is operated by the driving force of the motor 122 via the transmission mechanism 123, and the IJC 120 is calibrated.
- suction of ink by an appropriate suction means provided in the head recovery device 126 or ink to the IJC 120 is performed.
- Ink ejection is performed by an appropriate pressurizing means provided in the supply path, and ejection recovery processing such as removal of the thickened ink in the nozzle by forcibly discharging ink from the ejection port is performed.
- IJC is protected by caving at the end of recording.
- Reference numeral 130 denotes a blade disposed on the side surface of the head recovery device 126 as a wiping member formed of silicon rubber.
- Blade 130 is held by blade holding member 130A in the form of a force cantilever, and, like head recovery device 126, is operated by motor 122 and transmission mechanism 123 to discharge IJC 120. The engagement with the surface is enabled. This allows the blade 130 to be moved along the IJC 120 movement path at an appropriate time during the IJC 120 recording operation or after the ejection recovery processing using the head recovery device 126. It is made to protrude, and to wipe off dew condensation, wetness, dust, etc. on the discharge surface of the IJC 120 as the IJC 120 moves.
- the printing apparatus has an electric signal applying means for applying an electric signal for ejecting ink to the recording head.
- an electric signal applying means for applying an electric signal for ejecting ink to the recording head.
- a recording apparatus not only the above-described embodiment of recording on recording paper, but also a textile printing apparatus for recording a pattern on cloth or the like is an embodiment thereof. In this printing apparatus, since it is necessary to perform high-speed recording on a very wide cloth, it is particularly desirable to apply a long and good recording head of the present invention.
- the present invention brings about an excellent effect particularly in an ink jet recording head and an ink jet recording apparatus of a type in which ink is ejected by thermal energy among ink jet recording methods.
- the typical configuration and principle are, for example, those performed using the basic principle disclosed in U.S. Pat. Nos. 4,723,129 and 4,740,796. I like it.
- This method can be applied to both so-called on-demand type and continuous type.
- the on-demand type it can be used for sheets and liquid paths holding liquid (ink).
- heat is applied to the electrothermal transducers. This is effective because it generates energy and causes the film to boil on the heat-acting surface of the recording head, resulting in one-to-one correspondence to this drive signal and the formation of bubbles in the liquid (ink).
- the driving signal is in a pulse shape, the growth and shrinkage of the bubbles are performed immediately and appropriately, so that the ejection of a liquid (ink) having particularly excellent responsiveness is more preferable.
- the pulse-shaped drive signal those described in US Pat. Nos. 4,463,359 and 4,345,262 are suitable. Further, when the conditions described in U.S. Pat. No. 4,313,124 of the invention relating to the temperature rise rate of the heat acting surface are adopted, it is more excellent. Recording can be performed.
- the configuration of the recording head includes a combination of a discharge port, a wave path, and an electrothermal converter (a linear liquid flow path or a right-angled liquid flow path) as disclosed in the above-mentioned specifications.
- the configurations using U.S. Pat. Nos. 4,558,333 and 4,459,600 which disclose the configuration in which the action portion is arranged in the bending region are also effective in the present invention.
- Japanese Unexamined Patent Publication No. 59-123670 discloses a method of using a common slit for a plurality of electrothermal converters as a discharge section of the electrothermal converter, and discloses a thermal energy converter.
- the present invention is also effective as a configuration based on Japanese Patent Application Laid-Open No. 59-138641, which discloses a configuration in which an opening for absorbing the pressure wave is made to correspond to the discharge section.
- a replaceable chip type recording head or the recording head itself which is attached to the main body of the device and enables electrical connection with the main body and supply of ink from the main body.
- the present invention can also be applied to a case where a cartridge-type recording head provided integrally with the camera is used.
- the recording mode of the ink jet recording apparatus is not limited to the recording mode of only the mainstream color such as black, and the recording head may be formed integrally or by a combination of a plurality of recording heads.
- the present invention is also very effective for an apparatus provided with at least one full-color color or a full-color color mixture.
- the ink is described as a liquid.
- the ink solidifies at room temperature or lower, and changes or liquids at room temperature. It is common to control the temperature of the ink by adjusting the temperature within the range of 70 and below to stabilize the viscosity of the ink.
- the ink may be in a liquid state when the recording signal is applied.
- the temperature rise due to thermal energy can be prevented positively by using it as the energy for changing the state of the ink from a solid state to a liquid state, or solidified in a standing state to prevent evaporation of the ink.
- the ink is liquefied by applying the thermal energy according to the recording signal, and the ink is liquefied and discharged as an ink liquid or solidified by the time it reaches the recording medium.
- the use of an ink having the property of being liquefied for the first time by thermal energy, such as the one that starts, is also applicable to the present invention.
- the ink is applied to a porous sheet concave portion or through-hole as described in JP-A-54-56847 or JP-A-60-71260. It may be configured so as to face the electrothermal converter while being held as a liquid or solid.
- Example 1 the configuration and effects of the present invention will be described with reference to examples, but the present invention is not limited to these examples.
- Example 1
- a polycrystalline silicon ingot as a starting material was prepared as follows. In other words, high-purity polycrystalline silicon produced by hydrogen reduction and precipitation reaction by thermal decomposition used in the production of single-crystal silicon was introduced into a quartz crucible, where it was heated to 144 ° C. After melting, the mixture was poured into a graphite mold and cooled to prepare a polycrystalline silicon ingot measuring 80 cm square. At this time, no release agent was used. Next, at a position where the average crystal grain size becomes 2 mm from this ingot, each of the ingots was formed into a plate shape with the dimensions shown in the respective columns of Samples No. 1 to No. 12 in Table 6. One was cut out with a multi-wire machine.
- Lapping was performed on each of the obtained 12 polycrystalline silicon plates. After removing about 30 im of the surface part by flattening and flattening, it was chamfered with an end beveling machine.
- the surface was polished with a single-side polishing machine manufactured by Speed Fam Co., Ltd. to finish the mirror surface substrate with a surface roughness of Rmax 150.
- the polishing was performed without adding the abrasive.
- the surface roughness of each polycrystalline silicon that is, the surface of the polycrystalline silicon substrate was measured by a substrate surface inspection device in the same manner as in Experiment D. surface defects, and confirmed to be one Z cm 2 or less at all the measurement points further laser Tech Co. smoothness of the surface of each polycrystalline silicon base, a non-contact type surface roughness measuring instrument Measurements were made using the test, and it was confirmed that no steps were generated.
- the thermal oxidation conditions at this time were as follows.
- each of the four substrates on which the SiO 2 layer was formed was subjected to a thermal aging treatment to smooth the steps on the surface of the SiO 2 layer.
- the conditions of the heat softening treatment were as follows.
- each of the remaining four polycrystalline silicon substrates was subjected to a thermal oxidation treatment by a pyrogenic method to form a SiO 2 layer as a heat storage layer on the polycrystalline silicon substrate. did.
- impurities were diffused into the formed SiO 2 layer.
- the thermal oxidation conditions and impurity diffusion conditions at this time were as follows.
- Diffuse source POC l 3 diffusion method: atmospheric thermal CVD method diffusion temperature: 1 0 0 0 e C
- the impurity concentration of P diffused on the surface of the polycrystalline silicon substrate under the above conditions was 1 ⁇ 10 21 atoms / cm 3 as a result of measurement by SIMS. Subsequently, this SiO 2 layer was formed. Each of the four substrates was subjected to a thermal softening treatment to smooth the steps on the surface of the SiO 2 layer.
- the conditions of the heat softening treatment at this time were as follows.
- Heat softening time 1 hour
- 3 / thermal oxide layer of m (S i 0 2 layer) 4 sheets of polycrystalline silicon base for Uz de to a liquid jet recording with a thermal storage layer (Sample No, 9 to N o. 1 2) obtained .
- the shape of the step on the surface of the heat storage layer was examined with a stylus roughness meter and evaluated.
- the measurement method and evaluation criteria for the step shape were as follows.
- Measuring position The intersection of the line segment that divides the short side of the base 150 mm into four and the line that divides each of the long sides 600 mm, 500 mm, 400 mm, and 300 mm into six equal parts 15 places in total.
- Pattern samples of the liquid jet recording head were prepared at a rate of 15 samples per substrate. For each of Samples N 0.1 to No. 12, one of the fifteen pattern samples produced was shifted in focus position due to the warpage of the substrate, and one for the discharge port pattern. However, the pass rate for exposure was calculated based on the criteria for rejecting when a pattern was missing, and for passing when no such pattern was found.
- the exposure pass rate was calculated in the same manner as in the example.
- Table 8 shows the obtained results. As is evident from the results shown in Table 8, a decrease in the exposure pass rate was observed in Comparative Sample No. 2, and the majority of Comparative Sample No. 1 failed. Comparative samples Nos. 3 and 4 having short lengths exhibited an exposure pass rate of 100%.
- Example 2
- each of the 12 liquid jet recording head substrates (samples No. 1 to No. 12) shown in Table 6 prepared in Example 1 was used, and the following method was used.
- 15 liquid jet recording heads each having the configuration shown in the cross-sectional view of Fig. 3 were manufactured.
- a plurality of ink flow paths are formed on a liquid jet recording head substrate by photolithography using a photosensitive dry film, and then cut with a slicer to separate heads and form discharge ports. Was done.
- the outlet surface was polished to correct defects such as chipping that occurred during cutting.
- liquid jet recording head substrate fifteen liquid jet recording head in-process products were created.
- a heating resistor driving IC was connected to each of these 15 work-in-progress products and wiring using a flip-chip connection method, and a liquid jet recording head with a discharge port pitch of 63.5 m was created. .
- liquid jet recording heads of samples No. 1 to No. 12 15 liquid jet recording heads were created for each of the substrates.
- a group consisting of 15 liquid jet recording heads obtained from each of the samples No. 1 to No. 12 will be referred to as samples N 0.1 ′ to No. 12 ′, respectively.
- the production process yield of the liquid jet recording heads of the samples No. 1 'to No. 12' should be better than the predetermined ratio determined by the number of discharge ports. ⁇ , those which were worse than this ratio were evaluated as X and are shown in Table 7. In all of the liquid jet recording heads of the samples No. 1 'to No. 12', the occurrence state of the defect rate was within a predetermined level.
- V th is the foaming voltage
- the evaluation in the durability test was performed as follows. That is, the accumulated number of drive pulses is not broken for the total number of remaining rate, namely the heating resistor of the heating resistor when it becomes respectively 1 X 1 0 7, 1 X 1 0 8, 3 X 1 0 8
- the durability of the liquid jet recording head was evaluated by determining the number of heating resistors. Table 7 shows the obtained results. As apparent from the results shown in Table 7, in 3 X 1 0 8 times even residual rate after repeated in the discharge durability in 1 0 0% no problems result in even drive pulses each case there were.
- the ink composition used is as follows.
- Dye C.I. Direct black 19 3 wt%
- Heating resistor applied voltage 1.1 V th, (V th is foaming voltage)
- Driving frequency ⁇ ⁇ ⁇ ⁇ (heating resistor applied interval)
- Pulse width 10 s (1 pulse application time of heating resistor) Table 7 shows the print width in each liquid jet recording head. The printing samples obtained here were evaluated for printing accuracy and printing density unevenness as described below.
- the printing dot interval (dot center interval) of the printing sample was measured using a magnifying glass with a microscopic scale, and the range of the variation was determined.
- One measurement range was set to 2 cm square, and measurement was performed by selecting any 10 places on the printed sample.
- X is the paper feed direction and the vertical direction
- Y is the paper feed direction.For all 10 locations, all X-dot and Y-dot intervals of 2 cm square in the measurement range are in the range of 43.5 to 83.5 ⁇ m. Those in the list passed.
- the density unevenness of the printed sample was measured using a Macbeth densitometer.
- the entire surface of the print sample was read by a CCD scanner, and the optical density was measured for each 1 cm width in the direction perpendicular to the paper feed direction. A sample in which the optical density of an adjacent area on the entire surface of the print sample was within 0.2 was judged to be acceptable.
- ⁇ Non-defective liquid jet recording head is very slight and impractical.
- ⁇ When the yield does not exceed the expected yield based on the number of nozzles. The following can be understood from the results shown in Table 9. That is, in the case of the comparative sample No. 1 ′, a practically usable liquid jet recording head cannot be created. In the case of the comparative sample No. 2 ', the production yield of a practically usable liquid jet recording head is extremely low. The comparative samples No. 3 'and No. 4' have no problem in production yield.
- the headunit was prepared as follows. That is, a support member made of aluminum was used, and the first liquid jet recording head was fixed to one surface of the support member. Next, the second head was arranged and fixed on the other surface of the support member so that the arrangement interval of the discharge ports was as constant as possible over the entire length of the wave jet recording head including the connection area. .
- the comparative sample N 0. 'Of the head jet recording head thus obtained, an ejection durability test and evaluation of printing accuracy and density unevenness were performed in the same manner as in Example 2. The discharge endurance test passed, but the print accuracy was rejected due to the assembly error of the connection between the two heads. The density unevenness was rejected due to the difference in Vth (foaming voltage) between the two heads.
- FIG. 1 (A) is a schematic plan view of a main part of a liquid jet recording head substrate according to an embodiment of the present invention.
- FIG. 1 (B) is a cross-sectional view of an essential part taken along line XX ′ of FIG. 1 (A).
- FIG. 2 is a schematic cross-sectional view of a base constituting a liquid jet recording head substrate.
- FIG. 3 is a schematic cross-sectional view illustrating an example of manufacturing a liquid jet recording head.
- 4 (A) to 4 (C) are diagrams illustrating the formation of a thermal oxide film on the surface of a polycrystalline silicon substrate.
- FIG. 5 (A) is a cutaway perspective view of a main part of the liquid jet recording head.
- FIG. 5 (B) is a vertical sectional view of a main part of the liquid jet recording head in the flow path direction.
- FIG. 6 is a diagram showing an example of a recording apparatus provided with the liquid jet recording head of the present invention.
- FIG. 7 is a diagram showing an example of a thermal oxidation device for thermally oxidizing the surface of a base constituting a liquid jet recording head substrate.
- FIGS. 8 (A) and 8 (B) are views for explaining the mechanism of warpage occurring in the base.
- FIGS. 9 (A) to 9 (C) are diagrams illustrating the state of warpage occurring when the base is cut off.
- FIG. 9 (D) is an explanatory view of a method for measuring the degree of warpage of the substrate.
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/084,264 US5469200A (en) | 1991-11-12 | 1992-11-12 | Polycrystalline silicon substrate having a thermally-treated surface, and process of making the same |
EP92923536A EP0583474B1 (en) | 1991-11-12 | 1992-11-12 | Polycrystalline silicon-based base plate for liquid jet recording head, its manufacturing method, liquid jet recording head using the base plate, and liquid jet recording apparatus |
DE69219770T DE69219770T2 (de) | 1991-11-12 | 1992-11-12 | Polykristalline silicium enthaltende grundplatte für einen flussigkeitsstrahlaufzeichnungskopf, sein herstellungsverfahren, flussigkeitsstrahlaufzeichnungskopf damit versehen, und flussigkeitsstrahlaufzeichnungsgerät |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP29585291 | 1991-11-12 | ||
JP3/295852 | 1991-11-12 |
Publications (1)
Publication Number | Publication Date |
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WO1993009953A1 true WO1993009953A1 (en) | 1993-05-27 |
Family
ID=17826027
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP1992/001482 WO1993009953A1 (en) | 1991-11-12 | 1992-11-12 | Polycrystalline silicon-based base plate for liquid jet recording head, its manufacturing method, liquid jet recording head using the base plate, and liquid jet recording apparatus |
Country Status (4)
Country | Link |
---|---|
US (1) | US5469200A (ja) |
EP (1) | EP0583474B1 (ja) |
DE (1) | DE69219770T2 (ja) |
WO (1) | WO1993009953A1 (ja) |
Cited By (1)
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CN114295705A (zh) * | 2020-09-22 | 2022-04-08 | 苏州传澈特种材料有限公司 | 一种痕量检测方法 |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2933429B2 (ja) * | 1991-11-06 | 1999-08-16 | キヤノン株式会社 | 液体噴射記録ヘッド用基板、液体噴射記録ヘッドおよび液体噴射記録装置 |
JP3053936B2 (ja) * | 1991-12-04 | 2000-06-19 | キヤノン株式会社 | 液体噴射記録ヘッド用基体、該基体の製造方法、該基体を用いた液体噴射記録ヘッド、該記録ヘッドの製造方法及び該記録ヘッドを具備する記録装置 |
US5831648A (en) * | 1992-05-29 | 1998-11-03 | Hitachi Koki Co., Ltd. | Ink jet recording head |
JP3573515B2 (ja) * | 1995-03-03 | 2004-10-06 | 富士写真フイルム株式会社 | インク噴射記録ヘッド、記録装置、およびインク噴射記録ヘッドの製造方法 |
US5774148A (en) * | 1995-10-19 | 1998-06-30 | Lexmark International, Inc. | Printhead with field oxide as thermal barrier in chip |
JP3194465B2 (ja) * | 1995-12-27 | 2001-07-30 | 富士写真フイルム株式会社 | インクジェット記録ヘッド |
US6238041B1 (en) * | 1996-06-26 | 2001-05-29 | Canon Kabushiki Kaisha | Heat-generator supporting member for ink-jet head and ink-jet head employing the same |
US5943076A (en) * | 1997-02-24 | 1999-08-24 | Xerox Corporation | Printhead for thermal ink jet devices |
US6013160A (en) * | 1997-11-21 | 2000-01-11 | Xerox Corporation | Method of making a printhead having reduced surface roughness |
US6523938B1 (en) * | 2000-01-17 | 2003-02-25 | Hewlett-Packard Company | Printer orifice plate with mutually planarized ink flow barriers |
CA2377892C (en) * | 2000-05-11 | 2009-02-03 | Tokuyama Corporation | Polycrystalline silicon, method and apparatus for producing the same |
US7922814B2 (en) * | 2005-11-29 | 2011-04-12 | Chisso Corporation | Production process for high purity polycrystal silicon and production apparatus for the same |
US8960657B2 (en) | 2011-10-05 | 2015-02-24 | Sunedison, Inc. | Systems and methods for connecting an ingot to a wire saw |
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JPS59224358A (ja) * | 1983-05-25 | 1984-12-17 | Yokogawa Hewlett Packard Ltd | 熱インク・ジエツト・ヘツド |
JPS63228730A (ja) * | 1987-03-18 | 1988-09-22 | Matsushita Electric Ind Co Ltd | 半導体集積回路の製造方法 |
JPH03227634A (ja) * | 1990-02-02 | 1991-10-08 | Canon Inc | インクジェット記録装置 |
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US3887733A (en) * | 1974-04-24 | 1975-06-03 | Motorola Inc | Doped oxide reflow process |
US4535343A (en) * | 1983-10-31 | 1985-08-13 | Hewlett-Packard Company | Thermal ink jet printhead with self-passivating elements |
US4676868A (en) * | 1986-04-23 | 1987-06-30 | Fairchild Semiconductor Corporation | Method for planarizing semiconductor substrates |
EP0304337B1 (en) * | 1987-08-20 | 1994-10-05 | Canon Kabushiki Kaisha | Hybrid substrate |
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1992
- 1992-11-12 DE DE69219770T patent/DE69219770T2/de not_active Expired - Fee Related
- 1992-11-12 WO PCT/JP1992/001482 patent/WO1993009953A1/ja active IP Right Grant
- 1992-11-12 US US08/084,264 patent/US5469200A/en not_active Expired - Fee Related
- 1992-11-12 EP EP92923536A patent/EP0583474B1/en not_active Expired - Lifetime
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JPS59224358A (ja) * | 1983-05-25 | 1984-12-17 | Yokogawa Hewlett Packard Ltd | 熱インク・ジエツト・ヘツド |
JPS63228730A (ja) * | 1987-03-18 | 1988-09-22 | Matsushita Electric Ind Co Ltd | 半導体集積回路の製造方法 |
JPH03227634A (ja) * | 1990-02-02 | 1991-10-08 | Canon Inc | インクジェット記録装置 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114295705A (zh) * | 2020-09-22 | 2022-04-08 | 苏州传澈特种材料有限公司 | 一种痕量检测方法 |
Also Published As
Publication number | Publication date |
---|---|
DE69219770D1 (de) | 1997-06-19 |
US5469200A (en) | 1995-11-21 |
DE69219770T2 (de) | 1997-11-13 |
EP0583474A4 (en) | 1994-07-06 |
EP0583474A1 (en) | 1994-02-23 |
EP0583474B1 (en) | 1997-05-14 |
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